Copolymers for prevention of deposits in water-bearing systems, their preparing and using

FIELD: chemistry of polymers, chemical technology.

SUBSTANCE: invention relates to copolymers consisting of monomers comprising acid groups with double bond and other hydrophobic monomeric component used in prophylaxis of inorganic and organic deposits in water-bearing systems. Invention describes a water-soluble copolymer comprising: (a) monoethylene-unsaturated monomers chosen from group consisting of monocarboxylic acids, dicarboxylic acids and sulfoacids that can be neutralized; (b) at least copolymerizable hydrophobic acrylic, monocyclic and/or bicyclic terpene comprising unsaturated double bond wherein terpene hydrocarbon is preferable, and copolymer is prepared by free-radical copolymerization of components (a) and (b) in an aqueous phase. Also, invention describes a method for synthesis of abovementioned copolymer and methods for its using. Invention provides synthesis of nontoxic copolymer used for prevention of deposits in water-bearing systems that can be easily prepared from available components and able to store for a long time without loss of activity.

EFFECT: improved preparing method, valuable properties of copolymers.

22 cl, 6 tbl, 6 ex

 

The invention relates to copolymers containing acid groups of the monomers with double bonds, and other hydrophobic monomer component for the prevention of organic and inorganic sediments in the aquifer systems, and the way they are received.

Aquifers as a water and sewer system, cooling or heating circuits, systems, lubricating fluids, drilling fluid or process water for mass transfer, contain many microorganisms, such as bacteria of the species Pseudomonas vesicularis, Enterobacter cloacae, Citrobacter freundii and Enterobacter amnigenus, which occur in these systems rapidly grow. Due to reproduction and metabolism of microorganisms therefore, in these environments may be formed of biological masses, the so-called extracellular polymeric substances with inorganic multivalent cations often form gels and stick to the parts of plants.

In pipelines deposits can lead to a distinct drop in pressure which occur disproportionately narrowing cross-section. Further, these deposits can accelerate the corrosion of parts of plants, because the gels locally different oxygen concentration, redox potential, salinity and conductivity p the relation to the rest of the environment. If such deposits are formed larger education, there is a danger that they are separated and disrupt aggregates and mass production.

In cooling circuits deposits represent the insulating layer, which can greatly reduce heat transfer efficiency, so as to place deposits instead of the convective heat transfer occurs diffuse the heat transfer. You should indicate that organic contamination have clearly stronger insulating effect than inorganic raids.

Of particular importance are a mixture of organic and inorganic deposits, organic deposits create good conditions for growth and life in prevailing on the surface of the inorganic raids.

Especially in the case of paper production to prevent these biological processes of growth in the manufacturing process, which currently use bactericides (biocides, slimicides) based on the intensively active toxic substances.

Along with the problems that are associated with the safe handling and transportation of such toxic substances and limit the impact on the desirable scope of some of these bactericides should be used in combination and sequentially one after another to prevent the ustoichivosti microorganisms directly to the product. Besides the killing of microorganisms at the same time does not mean that they are removed from the system. Often remains dead biomass, which is a power source for subsequent microorganisms. Sediments are also a barrier in relation to biocides and can effectively protect them from intrusion. Therefore, this kind of gels and deposits strongly you want to delete from the system.

In the International application WO-95/15296 describes emulsions of the type oil-in-water, which prevent the formation of mucus in the aquifer systems. These emulsion of the type oil-in-water consist of a hydrophobic phase (oil phase), at least one emulsifier and water and their hydrophobic phase containing a biologically active substance, which may be acyclic, monocyclic and/or bicyclic terpenes, in particular terpene hydrocarbon. The disadvantage is that you can only prevent inorganic raids and we are talking about the emulsion.

The specialist knows that the emulsion, depending on the manipulation with them, the temperature and duration of storage, prone to delamination, due to which there is loss of action.

Along with organic sediments due to microbial processes in the aquifer systems in the manufacture of paper, particularly in the recycling of waste paper and manufactured and recycled paper, deposits will form, consisting of resins and residues of adhesives. These deposits can also occur when the system does not contain any microorganisms. The negative impact on parts of plants and the whole process is similar to the above.

In U.S. patent 5863385 describes the use of the emulsions of the type oil-in-water according to International application WO-95/15296 for the purpose of processing machines for the production of pulp, paper and cardboard to clean these units from adhering impurities from natural resins and/or synthetic polymers, as well as to prevent clogging of these aggregates such pollution.

In U.S. patent 5916857 describes how to remove sticky residues of resins in the case of paper machines with a cleaning tool consisting of a mixture of aliphatic petroleum distillates, d-limonene and esters of aliphatic dicarboxylic acids.

Along with just described deposits of organic origin and composition, the aquifer systems may appear inorganic sediments formed from salts and compounds used for the ongoing process water. In particular it should be called chlorides, sulfates, phosphates and carbonates of alkaline-earth metals. Some of these cations and anions can form insoluble salts or oxides, and the Hydra is xidi, which precipitate when exceeding the corresponding solubility products. In particular, soluble carbonates when heated become carbonates, and at elevated temperatures part of calcium salts precipitated as insoluble calcium carbonate. At high concentrations of magnesium may precipitate the carbonates of magnesium or, when appropriate pH value, also hydroxides. Known issue concerning the appearance of the residue in plants for wastewater treatment is the formation of magnesium ammonium phosphate. Other possible deposits are composed of calcium sulfate, silicates and phosphates in various forms in accordance with system conditions, such as pH value, temperature and degree of supersaturation, prone to the formation of plaque.

In the manufacture of paper it is necessary to specify the raids of calcium oxalate, because oxalic acid is present in the wood and is formed during the bleaching process due to the oxidative degradation of lignin and mono-, oligo - or polysaccharides, such as xylan.

Substances that prevent the precipitation of insoluble compounds, well-known specialist as a so-called stabilizers curing; for example, it should be called inorganic polyphosphates, ligninsulfonate is you, condensation products of naphthalenesulfonate, phosphonic acid, aminomethylphosphonic acid, esters of phosphoric acid, phosphonobutane acid, and polycarboxylic acids, such as partially saponified polyacrylamide or polymers, respectively, copolymers of acrylic acid. The lack of these substances is that some of these agents are toxic and can prevent only the inorganic sediment.

Along with attacks from directly formed insoluble inorganic compounds already present in the cooling system of the insoluble particles can lead to raids. This second large group forming raids inorganic components are suspended solids, which are derived from system or data entered into the system due to air in the case of an open cooling systems. Suspended solids are subjected to sedimentation in places with very low flow velocities in the system. Thus the resulting films may be formed of corrosion products raw materials, washed away the dust and solids from the added water. Next, can also form mixed sediments, which consist of sludge and precipitation of salts causing water hardness./p>

Already well-known products, often from a group of polymers, which act as dispersing agents, i.e. they stabilize microdisperse distributed particles of solids from sedimentation and sludge. In this case, use a polycarboxylic acid, such as partially saponified polyacrylamide or polymers, respectively, copolymers of acrylic acid with various comonomers, and polystyrenesulfonate, polyphenylsulfone, Quaternary ammonium compounds, neomillennial of polyacrylamide and polyalkylene glycols. The prior art disclosed in the following, among others, the following documents: the application for the European patent EP 8184223 A1, U.S. patent 4455235, patents great Britain 2105319 and 2152919. The disadvantage is that now you can avoid only the inorganic sediment.

The specialist knows that the aquifer systems in the chemical nature of the sediments is often uncertain and varies due to seasonal climatic changes. Due due to temperature fluctuations in the concentration of dissolved gases also change the content of soluble salts of water hardness. Climate due to seasonal fluctuations is exposed to the concentration of microorganisms. So it may be that in an industrial setting you want to avoid the season is about due to a variety of sediments, it is necessary to take various measures. During periods of changing weather conditions, winter - summer, and Vice versa, it is especially critical.

Therefore, there are also attempts to suppress the formation of deposits at the same time through the use of polymers and biocides, as described in European patent EP 892838 B1 or International application WO-96/14092. Also in the case of this method, the negative is the manipulation of toxic or hazardous biocides.

In U.S. patent 5756624 describes ternary copolymers on the basis of terpenes consisting of at least 10% of terpenes and other monomers from the group containing a double bond monocarboxylic acids with 3 to 5 carbon atoms and their esters, which get in the way of polymerization in mass. The disadvantage is that in case a specified polymerization without solvent reaches, in particular, high temperatures, due to what occurs undesirable staining of the product. Next, the thus obtained polymers are insoluble in water, in extreme cases, dispergiruyushchimi it. Proposed application, in particular, as modifiers of stickiness for adhesives and as modifiers.

In Eur. Polym. J., 24 (5), 453-456 (1988) also describes the radical copolymerization of terpene with maleic acid anhydride. These reactions are carried out in the form of polymerization of the solution, for example, tetrahydrofuran, benzene, dioxane or toluene. These partly poisonous and carcinogenic solvents should then be removed at considerable expense. The polymerization mass is not described.

The invention therefore is to obtain substances, compositions respectively, to prevent the formation of deposits in the aquifer systems and the method of production thereof, which possess no toxicity compared to known used still means are easily formed from just the available components and can be preserved for a long period of time without loss of activity. On the basis of application of the aquifer systems should be given whenever possible solubility in water. Efficiency should be as against inorganic and also against organic sediments and in particular also against combinations of both types of deposits. Then, inevitably must be reliable prevention of the sedimentation of solids in the system conditions. Along with this, a stabilizing and dispersing action of the substance, respectively, the composition should have an impact on equally and regardless of seasonal temperature fluctuations.

The task according to the invention is solved by obtaining water-soluble copolymers of

a) containing kislotno the e group of monomers with double bonds and

b) at least one of the following containing the double bond, copolymerizate hydrophobic components:

B1) acyclic, monocyclic and/or bicyclic terpenes, in particular, terpene hydrocarbons;

B2) unsaturated, open-chain or cyclic, normal structure or isomeric hydrocarbons from 8-30 carbon atoms;

B3) an unsaturated fatty alcohol or unsaturated fatty acids, respectively, with 8-30 carbon atoms and esters and amides of saturated aliphatic alcohols, amines and acids;

characterized in that the copolymers are formed by radical copolymerization of components (a) and (b) in the aqueous phase.

Proposed according to the invention the copolymers in comparison with the products according to the prior art, unexpectedly turned out to be soluble in water, the solutions are colorless and transparent. They can prevent not only the formation of both inorganic and organic deposits, but they also have distinctly improved properties compared with the pure polyacrylate while preventing the formation of inorganic deposits. The products are also particularly suitable for the prevention of mixed organic and inorganic deposits.

Moreover, these products are also extremely suitable for use PR is against microorganisms in aqueous systems, as, for example, in the case of sugar production from sugar beets or in the case of water circulation in the manufacture of paper or in clarifying installations.

Used according to the invention, containing acid groups, unsaturated monomers a) are monocarboxylic acids, such as acrylic acid, methacrylic acid, crotonic acid, Sekretareva acid, feniluksousna acid, partial esters of maleic acid, partial amides of maleic acid; dicarboxylic acids, such as maleic acid, fumaric acid, taconova acid; sulfonic acids, such as, for example, vinylsulfonate, arylsulfonate, metaliconfactory, 2-acrylamide-2-methyl-1-propanesulfonate, as well as their alkali metal salts and/or ammonium. Monocarboxylic acid preferably selected from the group consisting of acrylic acid, methacrylic acid, and sulfonic acids are preferably chosen from the group consisting of vinylsulfonate, (meth)arylsulfonate and 2-acrylamide-2-methyl-1-propanesulfonate.

From monocarboxylic acids are particularly preferred acrylic acid and its alkali metal salts and/or ammonium, and mixtures thereof. According to the following preferred variant implementation, monocarboxylic acid and containing sulfonylurea group monomers, as well as the x alkali metal salts and/or ammonium are used together, moreover, the share containing sulfonylurea group of monomers comprises from 0.1 wt.% up to 40 wt.%, preferably from 1 wt.% up to 25 wt.%.

Acid groups in the proposed according to the invention the copolymers neutralized, in General, 1-75%, preferably 2-50%, and particularly preferably 5-30%. They are preferably in the form of salts of alkali metals or ammonium.

As the hydrophobic component (b)in the case of B1), for example, should be called natural and synthetic terpenes, such as, for example, pinene as α-pinene and β-pinene, terpinol, lemon (dipentene), β-terpinen, γ-terpinen, α-Tuyen, Sabine, Δ3-Karen, camphene, α-cadinen, β-caryophyllene, adren, Balboni as α-Boulbon, β-Boulbon, γ-Boulbon, tsingiberen, Humulin (α-carioti-1-ene), α-citronellol, linalool, geraniol, nerol, ipsenol, α-terpineol, D-terpineol-(4), dihydrokavain, nerolidol, farnesol, α-eudesmol, β-eudesmol, citral, D-citronellal, carvon, D-pulegone, piperitone, Karvinen, bisabolene, β-salinan, α-sandalen, vitamin a, abietic acid and mixtures of these funds, as well as extracts from natural sources, such as, for example, present in orange terpenes. From terpenes preferred pinene, nerol, citral, citronellal, camphene, limonene/dipentene and linalool. Especially preferred limo is Yong/dipentene and pinene.

As the unsaturated hydrocarbons in the case B2), for example, you need to call the mission hexadecan, in case B3), for example, need to call monoalkyl a fatty acid ester, fatty acid amide or monoalkylated unsaturated fatty acids, mono - or polyesters of unsaturated fatty acids with polyols, with the exception of polyethylene glycols, mono - or polyamide, unsaturated fatty acids and aliphatic polyamines with the number of nitrogen atoms from two to six, oleic acid, oktilovom ester of oleic acid, mono - and trioleate glycerin, sorbifolia.

As a particularly preferred copolymerizes component b) use of acyclic terpenes and/or monocyclic and/or bicyclic terpene hydrocarbon.

The proportion of the component b) in the copolymer is, in General, from 0.001 wt.% up to 50 wt.%, preferably from 0.01 wt.% up to 30 wt.% and particularly preferably from 0.2 wt.% to less than 20 wt.%.

For further modification of the properties of the polymer, along with the above monomers is optional, you can use up to 40 wt.% other, soluble in water curable mixture of comonomers), as, for example, acrylamide, methacrylamide, Acrylonitrile, ethoxylate (meth)allyl alcohol and monetary (meth)acrylic acid and alcohols or ethoxylates, such as, for example, hydroxyethyl(meth)acrylate, hydroxypropyl(meth)acrylic is t, methoxypolyethyleneglycol-(meth)acrylate. Other suitable monomers should for example be mentioned: N,N-dimethylaminoethyl(meth)acrylate, N,N-dimethylaminopropyl(meth)acrylate, N,N-dimethylaminoethyl(meth)acrylamide and N,N-dimethylaminopropyl(meth)acrylamide. The preferred application is found with N,N-dimethylaminoethylacrylate and N,N-dimethylaminopropylamine.

H2C=CR1-CO-X-R2-N(R3)3Y-,

where R1 means a hydrogen atom, methyl; R2 means (C2-C4)-alkylenes group; R3 means a hydrogen atom, (C1-C4)-alkyl group; X denotes an oxygen atom, NH; Y represents a chlorine atom, SO4.

Due to the reactions of hydrolysis of these other comonomers after polymerization, if necessary, can form acid groups.

The mass-average molecular mass Mwproposed according to the invention copolymers are the largest in the area less than or equal to 500000 g/mol, preferably less than or equal to 100000 g/mol and particularly preferably from 1000 g/mol to 10,000 g/mol.

The object of the invention, then, is the method of obtaining the proposed according to the invention polymers, which is characterized by the fact that water-soluble copolymers obtained by radical polymerization of the Monomeric components in the aqueous phase. The concentration of the monomers polymerized in aqueous mixtures status is made usually from 10 wt.% up to 70 wt.%, preferably from 20 wt.% up to 60 wt.%.

Monomeric components with acid groups (a) before polymerization can be partially or completely neutralized and neutralized preferably 1-50%, particularly preferably 5-20% of the monomers a). For neutralization is preferably used such grounds, which have no negative impact on the subsequent polymerization. Use preferably a solution of sodium hydroxide and/or potassium hydroxide and/or ammonia, particularly preferably sodium hydroxide solution. In principle, however, may find the use of other bases, such as aliphatic amines or aliphatic aminoalcohols.

According to a further variant of the implementation of the monomers with acid groups before polymerization is not subjected to neutralization. If it is desirable, in this case, the neutralization can be performed after the polymerization reaction.

According to a preferred variant of the method of the Monomeric components (b) introducing the polymerized mixture in the form of an emulsion of the type oil-in-water. The proportion of oil phase in the emulsion of the type oil-in-water ranges from 1 wt.% up to 90 wt.%, preferably from 1 wt.% up to 50 wt.% and particularly preferably from 5 wt.% up to 30 wt.%, in terms of the total weight of the emulsion. The preparation used according to the invention emulsions, especially the items stable emulsions of the type oil-in-water, it is known, for example, International application WO-95/15296. To do this, the oil component emuleret in water using known suitable emulsifier to obtain an emulsion of the type oil-in-water. Emulsifiers are chosen by a well-known specialist criteria.

For polymerization in the aqueous phase, with the aim of obtaining the proposed according to the invention copolymers used several ways, as, for example, polymerization in solution, inverse emulsion polymerization and inverse suspension polymerization. Preferably carry out the polymerization in solution. Polymerization in solution can be performed continuously or periodically.

In the case of adiabatic polymerization reactions in solution before the polymerization of the monomer solution is cooled to a temperature below 30°C, preferably below 20°C.

The polymerization reaction can be initiated by a variety of conditions, such as, for example, by irradiation of radioactive, electromagnetic, or ultraviolet rays, or by using a redox reaction of the two compounds, as, for example, hydrosulfite sodium persulfate or potassium ascorbic acid and hydrogen peroxide. Also as the initiator of the polymerization reaction can be used thermally initiated decomposition of the so-called radical initiator, as in the example, azobisisobutyronitrile, peroxydisulfate sodium tert-butylhydroperoxide or Dibenzoyl peroxide. Further, it is possible to combine several of the above methods. Preferably use water-soluble initiators.

Moreover, in the prior art can be found a wide range of changes in the ratios of concentrations, temperature, kind and amount of initiators, as well as additional catalysts.

To obtain the desired molecular weight of the polymers may be necessary to carry out the polymerization reaction in the presence of growth regulators chain, i.e. the usual agents of chain breakage. Suitable growth regulators chain are, for example, aldehydes as formaldehyde, acetaldehyde, propionic aldehyde, n-Butyraldehyde, Isobutyraldehyde, formic acid, ammonium formate, hydroxylamine, and the sulfate, chloride or phosphate; contains mercaptopropyl connection, as thioglycolate acid, mercaptopropionic acid, mercaptoethanol, mercaptopropanol, mercaptoethanol, mercaptohexanol, timaliinae acid, thiophenol, 4-tert-butylthiophenol, n-dodecylmercaptan and/or tert-dodecylmercaptan. Other examples of growth regulators chains are allyl alcohol, butanol, isopropanol, n-butanol, Isobutanol, glycol, glycerin, pentaerythritol, fosforova sour is a and its salts, as, for example, hypophosphite sodium. Growth regulator circuit, if their use is necessary, use amounts up to 30 wt.%, in terms of the monomers. Preferably the polymerization reaction is carried out in the presence of 0.5-15 wt.% containing mercaptopropyl growth regulator circuit, calculated on the monomers.

Additive monomer components in the curable mixture can be implemented in such a way that either enter all the monomers, however, is metered separately or partially or completely mixed. When choosing a suitable method shall be guided, among others, the concentration of monomer in the polymerized mixture, the amount of the polymerized mixture, and the speed with which component b) is incorporated in the copolymer.

For introduction into the polymer chain of the component (b) may be predominant added to the polymerized mixture of emulsifiers.

The pH value generated according to the proposed invention the method of polymer solutions to be installed using suitable bases, such as sodium hydroxide solution, potassium hydroxide solution, in the range from 1 to 10, preferably from 3 to 7 and particularly preferably from 2.5 to 3.5.

Proposed according to the invention the copolymerization in aqueous phase flows simply and without problems and leads to the formation of clear solutions that can be used be the highlight of the polymer. In contrast, if applicable, described in the prior art, methods of polymerization in polluting solvents, respectively, in the case of methods of polymerization in mass produced copolymers, which are highly colored, insoluble and, in extreme cases, are dispersed in water.

The application of the proposed according to the invention copolymers

Used according to the invention the copolymers, respectively, the solutions of the copolymers used as such or diluted with water or containing water and solvent mixtures. The addition of the copolymer in the aquifer system, you can choose any image, preferably carry out single or multiple or continuous addition in the places where there is high concentration of microbes or their products of metabolism. High accumulation of microbes occurs, for example, in the manufacture of paper, in the case of the tributaries of the mass of the parts of the paper or other recycled materials.

In the cooling system additive is carried out either directly in the system or in the extension of the water. Use in open and closed cooling circuits in various degrees of condensation, especially in the range from 1 to 15, and temperature depending on climatic conditions and methods range from 5°, 250°C. the scope of the pH values of p and these applications is approximately 4-12, add the amount proposed according to the invention the copolymer is from 0.1 ppm to 5000 ppm, preferably from 0.5 ppm to 1000 ppm, and especially preferably from 1 ppm to 100 ppm, in terms of the aquifer system.

If proposed according to the invention the copolymers used in the manufacture of paper, the content of component b) is preferably more than 10%, in the case of applications in the field of cooling water it is estimated less than 10%, preferably less than 5% and especially preferably less than 1%.

A further area of use of such substances is dispersing and grinding a variety of inorganic pigments for the paper industry and ceramic industry, building materials industry (for example, colored concrete) and the chemical industry. Also in the case of production of dyes for a variety of products used dispersers.

So for dispersing and grinding use from about 0.1 wt.% up to 5 wt.% disperser, calculated on the pigment, for example, in the case of dispersion of kaolin or calcium carbonate, and pH ranges from 6 to 10 and receive a so-called slurry with pigment content of 50 wt.% up to 80 wt.%. Suspensions have a range of viscosity, comprising preferably from 200 MPa·d is 1500 MPa· C.

When the grinding and dispersion of dye required is clearly higher amount of dispersant. So, in the case of disperse dyes used from 10 wt.% up to 50 wt.% dispersant, in terms of the proportion of the dye. Using the proposed according to the invention copolymers reach viscosity, which facilitates the injection of slurry in the spray drying process.

The following scope of products is to prevent the formation of deposits in municipal and industrial clarification and installations. The pH value in the case of these applications is approximately 4-12, the dosage of the product is from 0.1 ppm to 2000 ppm, preferably from 0.5 ppm to 500 ppm and especially preferably from 2 ppm to 100 ppm, in terms of the aquifer system. Temperature, depending on climatic conditions and parameters of the method, different and can be up to about 100°C.

In the case of detergents and cleaner and proposed according to the invention the copolymers used mainly in the main system component/cocomponent.

In the textile industry proposed according to the invention, the copolymers are used as when washing the raw fiber and textile products, bleaching, washing after dyeing and as a dressing.

In kouwen the th industry proposed according to the invention, the copolymers can be used as in the processing of raw animal hides, and also tanning and doublepane skin. Tanning of hides copolymers enhance the absorption of chromium skin, when doublepane they preferably have an effect on staining, filling and strength of the front side of the skin.

In the case of certain applications it is useful to add to the proposed according to the invention the solutions of copolymers of further quantities of terpenes, preferably in the form of an emulsion of the type oil-in-water.

The invention is illustrated by the following examples.

Test methods

1. A study in the dynamics of suppressing the formation of plaque

The measurement is carried out using the so-called RAS (a device for monitoring and measuring pressure).

Constant volume flow of 2 l/hour stoichiometric mixture solution of dihydrate of calcium chloride, respectively, of sodium bicarbonate in fully deionized water (calculated stiffness for calcium: 30 German degrees of hardness) is passed through in a heating bath temperature of 90°With spiral metal capillary (length: 1 m, inner diameter: 1.1 mm). Both solutions combine just before the capillary. Means for preventing plaque formation, while adding before the test solution of sodium bicarbonate.

A series of tests beginning is only with a dosage of 4.5 ppm means to prevent plaque formation (in terms of dry substance). The testing time is one hour. Once on the inner walls of the metal capillary formed raids, its inner diameter is reduced. Since, however, the pump serves a constant volume flow, the pressure in front of the metal capillary increases. The change in pressure is continuously measured and recorded by a chart recorder. If after the time of the test does not detect any plaque formation, the following test is carried out using a reduced dosage. The goal is to determine the dosage, which guarantees the formation of plaque. Tests are used to compare products, i.e. tests compare products should be implemented using the same capillary. In the case of a series of tests with one or more products chosen by the so-called standard product, which includes the results of a series of tests. For this test with that of the standard product used in the dosages.

Used to compare the scale factor is calculated as follows: test pressure product after 40 minutes divided by the pressure at test standard after 40 minutes. Of course both tests must be carried out with the same dosage.

2. The determination of the relative dispersal abilities towards kao the inu (DSC)

The test method used for determining the dispersing ability of polyelectrolytes in relation to the particles of polluting substances in the circulation of cooling water.

Implementation testing

In the beaker is weighed 1,170 g of kaolin (10000 ppm) and use the eyedropper to add 116 ml of deionized water. Then, using a magnetic stirrer at a speed of approximately 600 rpm was dispersed for 10 minutes. When this set value pH 8.5, using a 4%aqueous solution of sodium hydroxide. When continuously operating magnetic stirrer select the eyedropper 19 ml and applied to a chemical test tube up to a height of 13 see Then immediately using a syringe with a capacity of 2 ml with cannula taken approximately 1.5 ml of the dispersion. The cannula of the syringe should be submerged approximately 9-10 cm from the upper edge of the chemical tubes, i.e. approximately 6-7 cm from the top of the liquid level. Of the sampled immediately weighed 1,000 g in a beaker and diluted with deionized water. Measure the extinction of this sample (zero test; variance without dispersant in aging time 0). In the remaining dispersion type dispersant in amount equal to 20 ppm of dry matter. The sample was incubated for 5 hours and then carry out the selection, as already described above, one sample volume of approximately 1.5 ml and RA is billaut the same way. Also in the case of these samples immediately determine the extinction at 450 nm (the value for the sample).

Assessment

The relative dispersal ability after the aging time of 5 hours is obtained by comparison with zero breakdown, the extinction of which is equal to 100%. Values for the samples are then x %.

3. Apparatus for testing the formation of organic deposits

Flow cell

To determine the effectiveness of preventing the formation of organic raids carried out using flow cells by assessing sediments that occur in the sample to be tested from steel, and it should represent the scale in the production of paper.

The device consists of a chemical glass Erlenmeyer, which result in movement in the apparatus for shaking (mark GFL 3031) with a speed of 160 rpm. Chemical glass filled with water solution and thermostatic at a temperature of 45°S. Of chemical glass are both ends of the silicone hose (4 mm × 7 mm). Using a pump (Watson Marlow 313 S) in the hose set volume flow 80 ml / min. All are in circulation volume of 50 ml In the middle of the hose is part silicone hose size 10 mm × 15 mm, in which you have entered the test sample (15 mm diameter and 2 mm thick; stainless steel, HAST AISI 316L).

During the test the whole system support at a temperature of 45°C. Before each new test system components are carefully cleaned. Use water, prevailing in the respective setting for paper production. First to the water (factory Stora Enso Inkeroinen; selected 10.01.2002,; food packaging and graphic cardboard, partially coated, 30% of married and 70% of trimethylolpropane; the pH value of water is 6.5; process temperature 50-55° (C) add 200 ppm polymers described in the examples, respectively, in the comparative examples, and incubated for 20 hours while passing through the flow cell. After following the addition of 200 ppm survive in the next hour in a flow cell. Then the samples are examined under the scanning electron microscope and/or EPI-fluorescence microscope and compared, respectively, with each other in the number, size and shape of the deposits. Follow the assessment system such that the net sample is denoted by the numeral 1, is closest to the pure sample is denoted by the numeral 2, and so on. Thus it is necessary to take into account that in a series of comparative tests of the same water examined at the same time and in the same conditions.

4. Determination of the dispersive action of the dispersant in the case of a pigment suspension

This method SL is incorporated to determine the amount of the dispersant to the pigment suspension with a given pigment content (approximately 30-80%) and pH values.

In chemical beaker 600 ml placed 166 g of deionized water together with the desired amount of dispersant additives and sodium hydroxide to adjust the value of pH. When the stirring speed 4000 min-1portions contribute 434 g of the pigment. After making the total number of pigment continue stirring for 15 minutes at a rotation speed of 5000 min-1. Suspension is set a solids content of about 73%. After a mixing time of 15 minutes experience a sample of the solid content using infrared dryer and then the sample thermostatic at a temperature of 25°C. After that, measure the suspension viscosity using Brookfield viscometer at a speed of 100 min-1. This test is recommended around with 4 different concentrations of dispersant to determine the optimal dosage.

The sample suspension was diluted with deionized water at a ratio of 1:9 and measure the pH value.

5. Determining the suitability of auxiliary tools for grinding and dispersing with the purpose of obtaining a pigment suspension

As a device for testing serves as a laboratory bead mill "Dyno-Mill KDL-Spezial". A mixture of 638 g of deionized water together with the desired number of auxiliary tools for rasmalai the tion and dispersion and sodium hydroxide to adjust the value of pH pre-dispersed using a laboratory mixer. The resulting solids content in the suspension is in this case about 75 wt.%.

The product is then transferred to a laboratory ball mill and the mill and pump. Register the disk-rotation speed in m/s and the duration of grinding. After the selected amount of time the suspension thermostatic at a temperature of 20°C, transferred into the mixer and mix for two minutes at a rotation speed of 1000 rpm-1. Then measure the viscosity using a Brookfield viscometer and determine the pH value at 10%dilution.

In conclusion, determine the distribution of particles using sedimentation scales (sedigraph).

Description of trials

Comparative example 1

70 g of the terpenes contained in oranges, 5.0 g of hexadecanol, 30 g of 75%paraffin sulfonate, 7 g proteinopathies with 20 moles of ethylene oxide olejowego alcohol and 5 g proteinopathies with 3 moles of ethylene oxide lauric alcohol melt until a homogeneous mass and then heated with stirring to a temperature of 85°C. To this solution is slowly poured 383 g of a 27%aqueous solution of homopolymer acrylic acid (Mw2500). In terms of the amount of the terpene, by analyzing the equilibrium vapor by gas chromatography products in the e detect 90% of free terpenes.

Comparative example 2

70 g of the terpenes contained in oranges, 5.0 g of hexadecanol, 30 g of 75%paraffin sulfonate, 7 g proteinopathies with 20 moles of ethylene oxide olejowego alcohol and 5 g proteinopathies with 3 moles of ethylene oxide lauric alcohol melt until a homogeneous mass and then heated with stirring to a temperature of 85°C. To this solution is slowly poured 383 g of fully deionized water. The thus obtained emulsion at room temperature, thoroughly mixed with 348,84 g of 30%aqueous solution of homopolymer acrylic acid (Mw2500). In terms of the amount of the terpene, by analyzing the equilibrium vapor by gas chromatography in the product detect 90% of free terpenes.

Example 1

Into the flask for the implementation of polymerization (with a stirrer, a tube for gas inlet and reflux condenser) is placed to 73.55 g of water, 150,0 g of acrylic acid (AA) and 225 g of terpenes contained in oranges, in the form of an aqueous emulsion according to International application WO-95/15296 (terpene emulsion B)within one hour skip the nitrogen, initiate with a solution of 5.7 g of peroxydisulfate sodium in 10 g of water, 10 g of 35%hydrogen peroxide and 20 g of mercaptoethanol. Within 7 minutes raise the temperature from 20°92°C. since the maximum temperature is ture, continue stirring at an internal temperature of 92°C. After 20 minutes add 0.75 g of azobis(2-amidinopropane)dihydrochloride (in the form of a solution in 5 g of water) and refluxed for 3 hours. Using a 50%aqueous sodium hydroxide solution set the pH value equal to 2.5. Get a clear solution. In terms of the amount of the terpene, by analyzing the equilibrium vapor by gas chromatography, the product can detect less than 40% of free terpenes, i.e. more than 60% used terpene entered in the copolymerization reaction.

Comparative example 3

Similar terpene emulsion B according to International application WO-95/15296.

Comparative example 4

In this case, follow the procedure of example 15 according to the U.S. patent 5756624.

4A) Mass ratio of monomers in the obtained polymer (the anhydride of maleic acid (AMC)/terpenes contained in oranges) is 70%:30%.

4B) Mass ratio of monomers in the obtained polymer (the anhydride of maleic acid/terpenes contained in oranges) is 80%:20%.

In both cases, get a solid pasta brown color, which is insoluble in water. This paste, however, can be partially dissolved, respectively, to dispergirujutsja in an aqueous solution of sodium hydroxide. Use 20%water disperse the polymer.

Comparative example 5

A homopolymer of acrylic acid with the mass-average molecular mass Mw2500.

Example 2

Into the flask for the implementation of polymerization (with a stirrer, a tube for gas inlet and reflux condenser) is placed 415,6 g of water, to 188.8 g of acrylic acid, to 47.2 g metalinsulator sodium and 11.8 g of terpene in the form of an aqueous emulsion according to International application WO-95/15296 (terpene emulsion B)within one hour skip the nitrogen initiate using 8 g of peroxydisulfate sodium, 15 g of 35%hydrogen peroxide and 20 g of mercaptoethanol. Within 10 minutes raise the temperature from 25°to 84°C. since the maximum temperature, continue stirring at an internal temperature of 90°C. After 20 minutes add 1 g azobis(2-amidinopropane)dihydrochloride (in the form of a solution in 5 g of water) and stirred for 2 hours. Then add 15 g of 35%peroxide hydrogen and refluxed for 3 hours. Get a clear solution. By analyzing the equilibrium vapor by gas chromatography in the product find only 2 ppm of free terpenes, and the rest joined in the copolymerization reaction.

Example 3

Follow the procedure of example 2. Instead of terpenes in the form of an aqueous emulsion using 1.7 g contained in oranges of terpenes.

Comparative example 6

The copolymer is krylovii acid and 20 wt.% metalinsulator sodium (NaMAC); the mass-average molecular mass Mw1900.

Comparative example 7

Follow the procedure of comparative example 2, however, instead of homopolymer acrylic acid using the product according to comparative example 6.

Comparative example 8

Follow the procedure of comparative example 1, however, instead of homopolymer acrylic acid using the product according to comparative example 6.

The examples described above are illustrated by tables 1A - 2B.

td align="center"> 1,2
Table 1a
Example [P]/SP1SPP1SP3
[SP]
a similar patentEP 892838 B1 or WO-96/14092EP 892838 B1 or WO-96/14092WO-95/15296
molecular weight, GPC* (Mw)250025002500
the monomerAKAKAK
the proportion of terpenes from orange in the composition [%]146614
RMES, standard scale factor4,81,5<40 min
DSK [%]73788330
organic sediment241i
notethe separation of the phasesthe separation of the phasesa clear solutionemulsion
water solubleYesYesYesno
*: helpanimals chromatography

1,0
Table 1B
Example [P]/SpaSPbSP5
[SP]
a similar patentUSA 5756624USA 5756624.
Molecular weight, GPC* (Mw)not definednot defined2500
the monomerAMK/terpenesAMK/terpenesAK
the proportion of terpenes from orange in the composition [%]640
RMES, standard scale factor<40 min<40 min
DSK [%]323782
organic sediment241
notebrown dispersion in an aqueous solution of NaOHbrown dispersion in an aqueous solution of NaOHa clear solution
water solublepartiallypartiallyYes

Table 2A
Example [P]/SPSPSP
[SP]
a similar patentEP 818423 A1 USA 4455235similar ER 892838 B1 or WO-96/14092similar ER 892838 B1 or WO-96/14092
molecular weight, GPC* (Mw)190019001900
the monomerAK/NaMACAK/NaMACAK/NaMAC
the proportion of terpenes from orange in the composition [%]00,30,3
RMES, standard scale factor1,01,21,3
DSK [%]878585
notea clear solutiona cloudy solutiona cloudy solution

Table 2B
Example [P]/P2PZ
[SP]
molecular weight, GPC* (MW)19001900
the monomerAK/NaMACAK/NaMAC
the proportion of terpenes from orange in the composition [%]0,30,3
RMES, standard scale factor0,90,5
DSK [%]8685
notea clear solutiona clear solution

The test results on the dispersion of calcium carbonate

In the following table 3 presents the results regarding the effectiveness of using as a dispersant polymers according to examples 1 and 2 and comparative example 1.

Table 3
ProductDosage, %, dry substanceViscosity, MPa·s at 100 rpm Caso3, %PH
SP10,08630819,9
P10,08289819,9
P20,0848181the 9.7

Proposed in the invention, the polymers according to examples containing terpenes from orange are clearly the best dispersing impact than the copolymer according to the comparative example. Lower viscosity, in General, clearly indicates the dispersibility of the particles.

The test results for the grinding and dispersion of calcium carbonate.

In the following table 4 presents the effectiveness of the proposed according to the invention polymers as an aid for milling.

0,8
Table 4
ProductDosage, %, dry substanceViscosity, MPa·s at 100 rpmCaso3%PHParticles % <2 μmParticles % <1 μm
SP0,81850769,993,571,6
P11220769,8for 91.370,1
P20.895076the 9.7to 91.670,4

Proposed according to the invention polymers have very good behavior when used as auxiliary tools for milling. Compared with conventional polymer as auxiliary tools for milling, in the case proposed in the invention copolymers receive a distinctly lower viscosity of the pigment suspensions.

1. Water-soluble copolymer containing

a) monomethylethanolamine monomers selected from the group consisting of monocarboxylic acids, dicarboxylic acids and sulfonic acids, which may be neutralized,

b) at least copolymerizing hydrophobic acyclic, monocyclic and/or bicyclic terpene containing an unsaturated double bond, preferably terpene hydrocarbon,

characterized in that the copolymer obtained by free-radical copolymerization of components (a) and (b) in the aqueous phase.

2. The copolymer according to claim 1, characterized in that monomethylethanolamine monomers selected from the group consisting of acrylic acid, methacrylic acid, vinylalcohol acid, preferably krylovii acid.

3. The copolymer according to claim 1, characterized in that monomethylethanolamine the monomers are neutralized to 1-75%.

4. The copolymer according to claim 1, characterized in that monomethylethanolamine the monomers are neutralized by 5-30%.

5. The copolymer according to any one of claims 1 to 4, characterized in that the proportion of the component b) is from 0.001 to 50 wt.%.

6. The copolymer according to claim 5, characterized in that the proportion of the component b) is from 0.01 to 30 wt.%.

7. The copolymer according to any one of claims 1 to 4, characterized in that it contains additionally up to 40 wt.% not containing acid groups, water-soluble monomers).

8. The copolymer according to claim 5, characterized in that it contains additionally up to 40 wt.% not containing acid groups, water-soluble monomers).

9. The copolymer according to any one of claims 1 to 4, 6, 8, characterized in that it has a mass-average molecular mass of less than or equal to 500000 g/mol.

10. The copolymer according to claim 5, characterized in that it has a mass-average molecular mass of less than or equal to 500000 g/mol.

11. The copolymer according to claim 7, characterized in that it has a mass-average molecular mass of less than or equal to 500000 g/mol.

12. The copolymer according to claim 9, characterized in that it has a mass-average molecular weight of from 1000 to 10000 g/mol.

13. The method of obtaining water-soluble copolymer according to any one of claims 1 to 12, characterized in that the copolymer formed by free-radical polymers is the Monomeric components in the aqueous phase, and concentration copolymerizing components in the water of the polymerized mixture is from 10 to 70 wt.%.

14. The method according to item 13, wherein component b) is used in the form of emulsions of the type oil-in-water, which is formed from a hydrophobic phase (oil phase), at least one emulsifier and water.

15. The method according to item 13 or 14, characterized in that the radical polymerization is carried out in the presence of growth regulators chain.

16. The use of a copolymer according to any one of claims 1 to 12, to prevent the formation of organic, inorganic or mixed organic and inorganic sediments in the aquifer systems.

17. The use of a copolymer according to P16 in industrial or sewage systems, cooling circuits, units for desalination of sea water, reverse osmosis for treatment of brackish water and in the case of extracting sugar from sugar beet, in particular for the treatment of aqueous suspensions rugged sugar beet roots.

18. The use of a copolymer according to 17 in obtaining sugar from sugar beet for processing aqueous suspensions with the rugged sugar beet roots.

19. The use of a copolymer according to any one of claims 1 to 12 in an amount of from 0.1 to 5000 ppm to prevent the formation of organic, inorganic or mixed organic and inorganic, otlozhenii is in aquifer systems.

20. The use of a copolymer according to claim 19 in an amount of from 1 to 100 h/million

21. The use of a copolymer according to claims 1 to 12 as an aid in the grinding and dispersion of pigments.

22. The use of a copolymer according to claims 1 to 12 as an aid in the compositions of detergents and products for cleaning and treatment processes of textiles and leather.



 

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