Biologically compatible gel thickened with cross-linked polymer

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing biologically compatible gel which is thickened with cross-linked polymer by cross-linking a given amount of at least one biologically compatible natural polymer in a solution by adding a defined amount of cross-linking agent, an additional amount of polymer with molecular weight over 500000 dalton in a solution, in which the reaction mixture is diluted to reduce concentration of polymer in the solution, and the cross-linking reaction is stopped by removing the cross-linking agent.

EFFECT: gel and its use for separating, replacing or filling biological tissue or for increasing volume of such tissue, or supplementing or replacing biological fluid.

11 cl, 1 tbl, 4 ex

 

The present invention relates to a method for producing a thickened cross-linked biologically compatible polymer gel, said gel and its application to obtain a matrix comprising at least one dispersed the beginning of the current, or to replace or fill in biological tissue, or to increase the amount of this fabric, or other additions or replacement of body fluids.

The increase in the volume of tissue is desirable in the case of use in therapeutic and cosmetic purposes. It is carried out by introducing into tissue viscoelastic solution based on resistant or susceptible to biological decomposition of substances.

Injection of viscoelastic solution based on resistant or susceptible to biological decomposition of substances also provide for the replacement of body fluids.

The solution is applied, for example, for replacement in patients with osteoarthritis patients natural synovial fluid, no longer able to perform the functions of protection of cartilage, lubricate and absorb the shocks due to the decrease in the number and molecular weights of its constituent glycosaminoglycans. However, if this viscoelastic solution consists of exposed biological decay of substances, it is rapidly eliminated from the synovial sinus.

The use of viscoelastic solution of this type for medicinal purposes includes the use of to increase some tissues, in order to ensure the exercise of their functions; examples are the vocal cords, esophagus, urinary sphincter or the urethra.

The use of viscoelastic solution of this type for cosmetic purposes includes its use, for example, to eliminate wrinkles, scar camouflaging or lip augmentation. Injection of such viscoelastic fluids is a simple non-invasive procedure, coupled with less risk and less inconvenience than plastic surgery.

The advantage of viscoelastic solutions on the basis of persistent substances is that they for a long time remain in the tissues in which they entered.

For a long time it is known the use of silicone injections. However, given the undesirable remote consequences of this method in the appearance of the skin nodules and ulcers its use is gradually released from the practice.

Injection of solid particles in suspension also provides a persistent increase in the volume of tissue. In U.S. patent US 5344452 described the use of powdered solid substance consisting of small particles with a diameter of from 10 μm to 200 μm with a smooth surface. Commercially available products Artecoll® and Arteplast® represent a suspension of microspheres of polymethacrylate in a solution of collagen. In the European patent EP 1091775 proposed suspension of fragments g is dragula-based methacrylate in a solution of hyaluronate. Also known application of particles of silicone compounds, ceramic, carbon or metal (USA patent US 5451406, US 5792478 and patent application U.S. 2002-151466) and fragments of polytetrafluoroethylene, glass or synthetic polymers (patent application U.S. 2002-025340), but the results are disappointing. So, it is known that there may be adverse reactions, biological decay of the solution or are susceptible to biological degradation suspension and migration of residual fragments capable of causing an inflammatory response. In addition, the injection of particles at a thin needle may be difficult if the particles are too large a diameter or irregular shape, which can lead to sticking of the particles to each other. In addition, when the injection of fragile particles, their structure may be damaged, resulting in the injection of very small particles that do not interlock with adjacent cells, and migrate in the direction of other tissues or quickly subjected to fermentation by macrophages and other components of the lymphatic system.

In General, the resistance of these substances is the cause of serious shortcomings (U.S. patent US 6436424)associated with a substantial risk of activation of macrophages, migration of synthetic fragments forming substance with the ability Vozniknovenie the inflammatory response, which can even lead to granulomas. For the treatment of granulomas desired therapeutic steroid injections or surgical removal, which is associated with serious consequences for the patient's health or quality of life. Thus, adverse effects of persistent substances are so severe that they limit their use for purely cosmetic purposes. In addition, injection of viscoelastic solution on the basis of persistent substances does not allow corrections if they are needed.

Among the exposed to the biological decay of substances known to the suspension of crosslinked collagen or hyaluronic acid.

The company Collagen Corporation has developed a drug based on glutaraldehyde cross-linked collagen, which is described in U.S. patent US 4582640. However, when injected into the tissue due to the injection of this substance is rapidly decomposed under the action of macrophages or enzymatic or chemical attack, and then withdrawn from the tissue of the lymphatic system. In U.S. patent US 5137875 proposed the use of suspensions or aqueous solutions of collagen containing hyaluronic acid, but this substance is not capable of providing long-term therapeutic effect, because it quickly undergoes fermentation and subsequently eliminated by the lymphatic system. Therefore, repeated application that SV is connected with significant costs and impairs the patient's quality of life.

In the European patent EP 0466300 proposed injection biphasic viscoelastic gel, consisting of a matrix, dispersed in the liquid phase, and both phases are extracted from cross-linked high molecular giulana, hyaluronate animal origin. Application of high-molecular polymer allows for a long-term presence in the tissue of the subject to biological decay viscoelastic gel. The result of the development of this technology was the emergence on the market of certain substances, such as Hylaform® to fill depressions in the intercellular matrix of connective tissue or Synvisc®, which is the product of viscopaste for the treatment of arthritis.

From the number of exposed biological decay of the two-phase substances can also mention Restylane®, Macrolane®, Pelane® or Durolane®, other two-phase composition consisting of a liquid phase (not cross-linked hyaluronate) and phase comprising hyaluronic acid. In a basis of these substances, designed to increase tissue (face, breast cancer) or treatment of arthritis, based on the NASHA technology company Q-Med. It is established that under certain circumstances the use of two-phase substances can cause inflammatory reactions or even lead to the appearance of granulomas (Laeschke K., Biocompatibility of microparticles into soft tissues fillers. Congress of Aesthetic Medicine and Dermatologic Surgery, Paris, 2003) even with acetato, such reactions are less prominent than the presence of gel-based synthetic polymers. In addition, fluid phase is very rapidly excreted, resulting in a loss of substance in the volume of such fluid phase. As a result, when it is necessary to increase the amount of fabric required to make many corrections after the first injection, which impairs the patient's quality of life.

Finally, the known number of single-phase viscoelastic gels intended for homogenizing the degree of crosslinking of the gel (patent application U.S. 2003-148995) or regulation ability of the gel to biological degradation (U.S. patent US 4963666), or to regulate the viscoelastic properties of the gel (U.S. patent US 5827937). A high degree of crosslinking, provides a more long-term presence in the tissue of the subject to biological decay viscoelastic gel. However, injection of a gel consisting of such longevity highly crosslinked polymer, is more complex. In addition, the injection of such a gel is not cross-linked sites of the polymer acquire mechanical fragility, becoming more vulnerable to biochemical and enzymatic action, which contributes to the rapid collapse of the gel.

The objective of the invention is the creation of thickened cross-linked biologically compatible polymer gel without the above disadvantages, at the same time which is simple clinical PR is changing and in this lifetime, that thickened cross-linked biologically compatible polymer gel disappears when there is no need in his action, but enough to limit the number of applications through medical or surgical intervention.

To this end, in the invention, a method for obtaining a dense cross-linked biologically compatible polymer gel, namely, that provide the stage on which:

begin stitching the quantity, of at least one biocompatible polymer in solution by adding a certain amount of cross-linking agent,

- carry out the crosslinking reaction of the above mentioned amount of polymer,

- enter the extension number of polymer with molecular weight of over 500,000 daltons in a solution in which the reaction mixture is diluted to reduce the concentration of polymer in solution, and carry out the stitching, and

- stop the crosslinking reaction by removing the cross-linking agent.

By introducing an incremental amount of polymer creates a new reaction point.

The described method allows to obtain a thickened cross-linked biologically compatible polymer gel, which is also single-phase, dense polymer capable of coupling, injectable and capable of a long time to remain in the tissue.

The ability to grip Osnach is no property of the gel to regroup and not to rassredotochivaniya or decompose. Thus, the coupling provides high compatibility and long residence time of the gel in the tissue in vivo.

Thickening polymer means a change in the degree of crosslinking even within the gel. Thickening gel polymer allows the injection of the composition through a needle of small diameter and provides a long residence time of the gel in the tissue in vivo.

Odnofaznogo reduces the risk of inflammatory reactions and the appearance of granulomas.

The ability of the gel for a long time to be in the fabric allows you to distribute medical intervention in time and, consequently, to improve the quality of life of patients.

Capable of coupling gelled polymer monophasic gel obtained by the method according to the present invention differs lightweight ineterest and a longer residence time in the tissue compared with the single-phase gel of the same composition, the degree of crosslinking in which the gel is homogenized.

In the private embodiment of the invention stage of start stapling is carried out in an alkaline medium.

In another embodiment of the invention stage of start stapling is carried out in an acid medium.

According to the improvement of the invention at the stage of introduction of the incremental amount of polymer injected additional amount of the crosslinking agent.

Preferably, the stage stop stapling is carried out by dialysis. Dialysis provides the final termination of the reaction. When this occurs, the removal of cross-linking agent and did not participate in the reaction of short polymer chains.

It is desirable that the polymers had a natural origin. Through the use of a polymer of natural origin is improved biological compatibility, that is, reduces the risk of inflammatory reactions.

Preferably, the polymers of natural origin are compounds selected from the group comprising hyaluronic acid, chondroitin sulfate, keratan, Kermanshah, heparin, heparansulfate, cellulose and its derivatives, alginates, xanthan gum, carrageenin, proteins or nucleic acids.

More preferably, at least one polymer of natural origin represented the polymer, which by nature is not human organism selected from the group comprising cellulose and its derivatives, alginates, xanthan gum, carrageenin, a polymer made of at least one polymer, which by nature is present in the human body selected from the group comprising hyaluronic acid, chondroitin sulfate, keratan, Kermanshah, heparin, heparansulfate, proteins or nucleic acids.

Preferably, cross-linking the Gent was a two - or multi-functional molecule, selected from compounds of the group, including epoxides, epichlohydrin and diphenylsulfone.

The objective of the invention is a gel obtained as described above.

Preferably, the gel consists of a matrix that contains at least one active principle dispersed. The gel is subsequently used as a vector that provides a gradual release referred to the beginning of the current in the fluid or biological tissue into which it was injected with.

Finally, the invention is also the use of this gel for separation, replacement or filling of biological tissue or to increase the amount of this fabric, or addition or replacement of body fluids.

For a better understanding of the invention and other of its objectives, details, features and advantages hereinafter the invention is described with reference to its implementation, employee solely illustrating and not limiting the invention an example.

A method of obtaining a dense cross-linked biologically compatible polymer gel is characterized by the fact that consistently carry out the stage where you begin stitching a specified number of at least one biocompatible polymer in solution, carry out the crosslinking reaction of the above mentioned amount of polymer injected add the offered quantity of polymer with molecular weight of over 500,000 daltons in solution, in which the reaction mixture is diluted to reduce the total concentration of polymer in the solution, carry out the stitching and stop the crosslinking reaction by removing the cross-linking agent.

Start stapling is carried out by adding a certain amount of cross-linking substance, which is a two or multi-functional molecule selected from the group of compounds including epoxides, epichlohydrin and diphenylsulfone.

Preferably, the epoxides are compounds selected from the group comprising 1,4-potentialapplications ether (also called 1,4-bis(2,3-epoxypropoxy)butane), 1-(2,3-epoxypropyl)2,3-epoxycyclohexane and 1,2-ethiological ether.

In the private embodiment of the invention stage of start stapling is carried out in an alkaline medium. The crosslinking reaction taking place in an alkaline medium, is distinguished by the formation of ether linkages of high strength. By crosslinking through the formation of ethers increase the residence time in the tissue in vivo.

In another embodiment of the invention stage of start stapling is carried out in an acid medium. The crosslinking reaction taking place in an acid medium, is formation of a complex ester bonds, which are less stable than those mentioned ether linkages. However, the lower resistance of bridging ties is the procedure provides certain advantages. In particular, such a gel is used as a matrix containing dispersed active principle, has different kinetics of release of the current start, which is more acceptable in some applications.

The crosslinking reaction is a reaction that provides the formation of bridging ties between chains of molecules of each polymer. For its quantitative expressions determine the degree of crosslinking.

The degree of crosslinking is expressed as the relationship between the number of moles of a crosslinking agent, ensuring the formation of bridging ties between chains of molecules of each polymer, and the number of moles of polymer units.

Crosslinking occurs in the temperature range preferably from 25°C. to 60°C.

The stitching is performed with a single polymer or mixture of polymers.

The polymers involved in the crosslinking reaction are synthetic polymers, but preferably polymers of natural origin. Through the use of a polymer of natural origin is improved biological compatibility, that is, reduces the risk of inflammatory reactions.

Preferably, use of the above-mentioned polymers of natural origin.

However, it is obvious that the invention is not limited to the application of the above-mentioned polymers and can be used polymers of various types and RA is Mer.

Stage introduction of additional polymer accompanied by dilution of the reaction medium to reduce the total concentration of polymer in solution.

Under these conditions, the polymer chains new point of stitching, which react with the remnants of a crosslinking agent and/or added in a small amount of a crosslinking agent, gaining traction on the chains initially cross-linked gel and between them with a lesser degree of crosslinking, since the amount of crosslinking agent is decreased.

The number of bridge links on the chains of the gel formed in the first stage of the stapling exceeds the number of bridging ties between them and added chains and the number of bridging ties between the added circuits. Thereby vary the degree of crosslinking in the resulting gel is formed longevity highly crosslinked nodes (with degree of crosslinking, for example, 25%), the United gel with all the decreasing degree of crosslinking (degree of crosslinking which gradually decreases and can reach 1%). This feature gives the gel its exceptional viscoelastic properties, due to which the gel with a high degree of crosslinking and, therefore, a long time in tissues in vivo has the ability to grip (the same gel) and can be introduced by injection using medical devices of any kind, in particular onca needles.

Additional polymers injected at any point in the course of the initial crosslinking reaction, preferably after passing 75% of the original reaction stitching. This stage is carried out by continuous or intermittent addition of the polymer.

Additional polymers should have a molecular weight of over 500,000 daltons. They can also be synthetic, or have a natural origin. They are added in the form of a mixture of polymers. Their nature or size may be the same or different from the origin and size of the polymers used in the initial stage of stitching. It is advisable to put the extension polymers had a chain of greater length than initially present polymers. This improves the external mechanical structure of the gel, since longer chains are less prone to decay than short chains.

Accordingly, this method allows to obtain a thickened cross-linked biologically compatible polymer gel, which is also single-phase, gelled polymer, has the ability to grip is injectable and has a long residence time in the tissue.

In the private version of the invention, the additional amount of the crosslinking agent is injected at the stage of introduction of the additional polymer. The nature of this cross-linking agent may be the same or differ Atsa from the nature of the agent, used at the beginning stage of the reaction. It is preferably chosen from the compounds in the above-mentioned group. Added a number of mostly inferior to the number added during the initial stitching.

Stage termination reactions stitching is used for the final termination of the reaction. It, for example, is carried out by dialysis, which allows you to delete a crosslinking agent and did not participate in the reaction of short polymer chains. Injection of the gel containing the agent that causes inflammatory reactions, because these agents consist of hardly digestible chemical compounds have a high reactivity.

Preferably, the gel consists of a matrix containing at least one active principle dispersed. Thus, the gel is used as a vector that provides a gradual release referred to the beginning of the current in the fluid or biological tissue into which it was injected with. The active principle is a substance having a pharmacological action, such as an antioxidant. The active principle may also be of different nature. The gel can also be dispersed mixture of active principles of various nature.

This gel is preferably administered by injection.

Finally, the gel is desirable is used for separation, replacement or filling of biological tissue or to increase the volume of a tissue, for example, in the case of therapeutic use (increasing the volume of the vocal cords, esophagus, urinary sphincter, urethra or other bodies) or for cosmetic purposes to eliminate wrinkles, scar camouflaging or lip augmentation.

It can also be used to augment or replace biological fluids such as synovial fluid of the body.

To illustrate the invention, it is provided with examples, which in no way his limit.

Example 1 (comparative)

10 g of hyaluronic acid (molecular weight = 2×106daltons) was dissolved in 100 ml of 1% NaOH solution. At this stage, prior to stitching, hyaluronic acid was hydrational.

The resulting mixture was homogenized to obtain a clear solution.

Then to the solution was added 470 l 1,4-potentialapplications ether to give effect to a crosslinking reaction, and the mixture was stirred for 15 hours at a temperature of 25°C in an oxygen-free environment.

The pH brought to physiological using 1 M HCl. Using a buffer solution with pH=7 reduced mixture of 400 ml.

Then, the resulting gel was subjected to dialysis within 24 hours (regenerated cellulose, the limit of separation: molecular weight = 60 kelod is lton) using a buffer solution with pH=7 (gel I).

The total content of hyaluronic acid in the gel was 2.5 wt.%.

Example 2 (comparative)

The gel was obtained by the method of Example 1 except that there was added a greater amount of cross-linking agent.

10 g of hyaluronic acid (molecular weight = 2×106daltons) was dissolved in 100 ml of 1% NaOH solution.

The resulting mixture was homogenized to obtain a clear solution.

Then to the solution was added 760 l 1,4-potentialapplications ether to give effect to a crosslinking reaction, and the mixture was stirred for 15 hours at a temperature of 25°C in an oxygen-free environment.

The pH brought to physiological using 1 M HCl.

Using a buffer solution with pH=7 reduced mixture of 400 ml.

Then, the resulting gel was subjected to dialysis within 24 hours (regenerated cellulose, the limit of separation: molecular weight = 60 kilodaltons) using a buffer solution with pH=7 (gel II).

The total content of hyaluronic acid in the gel was 2.5 wt.%.

Example 3 (comparative)

The gel was obtained by the method of Example 1 except that there was added an even greater number of cross-linking agent.

10 g of hyaluronic acid (molecular weight = 2×106daltons) was dissolved in 100 ml of 1% NaOH solution.

The resulting mixture was homogenized to obtain the transparent the aqueous solution.

Then to the solution was added to 950 l 1,4-potentialapplications ether to give effect to a crosslinking reaction, and the mixture was stirred for 15 hours at a temperature of 25°C in an oxygen-free environment.

The pH brought to physiological using 1 M HCl.

Using a buffer solution with pH=7 reduced mixture of 400 ml and homogenized.

Then, the resulting gel was subjected to dialysis within 24 hours (regenerated cellulose, the limit of separation: molecular weight = 60 kilodaltons) using a buffer solution with pH=7 (gel III).

The total content of hyaluronic acid in the gel was 2.5 wt.%.

Example 4 (invention)

10 g of hyaluronic acid (molecular weight = 2×106daltons) was dissolved in 100 ml of 1% NaOH solution.

The resulting mixture was homogenized to obtain a clear solution.

Then to the solution was added to 950 l 1,4-potentialapplications ether to give effect to a crosslinking reaction, and the mixture was stirred for 9 hours at a temperature of 25°C in an oxygen-free environment.

Then introduced an extension of the polymer and brought the volume of the mixture to 300 ml using 0.5% solution of hyaluronic acid, pH=11 (molecular weight = 2×106daltons).

Continued reaction for 6 hours. Using 1 M HCl brought the pH to physiological and brought the volume of the mixture up to 400 m is.

The mixture is homogenized.

Then to finally terminate the reaction, crosslinking the obtained gel was subjected to dialysis within 24 hours (regenerated cellulose, the limit of separation: molecular weight = 60 kilodaltons) using a buffer solution with pH=7 (gel IV).

Only the last gel was obtained by the method according to the invention, whereas the gels of the other three types were obtained known from the prior art methods, i.e. using the uniform bound.

The total content of hyaluronic acid in the gel amounted to 2.75 wt.%.

The gels obtained according to Examples 1-4 were determined rheological properties.

For this measured maximum extrusion force (F) of the gel, i.e. the force with which the gel may be subjected to extrusion.

To this end, the gel was placed in a stainless cylinder with a diameter of 2.5 cm and subjected to extrusion through pores with a diameter of 0.2 mm the results are shown in the table below.

Table
The gel typeF (H/mm2) σ=0.15 N/mm2
Iof 3.56
II5,85
III 7,40
IV6,12
σ: standard deviation

Gels I, II and III are gels with a constant degree of crosslinking throughout the gel. Only gel IV is a gel with a variable degree of crosslinking.

Proposed in the invention method, first of all, demonstrated that as you add more and more cross-linking agent (gel types I-III) is also increasing maximum extrusion force, i.e. the force needed to apply for the extrusion of the gel with an increasing degree of crosslinking increases for gels with a uniform degree of crosslinking.

The injection of the gel type IV (gel according to the invention)containing a 2.75 wt.% hyaluronic acid, carry out almost as easily as gel containing 2.5 wt.% hyaluronic acid, the degree of crosslinking which is smaller and is uniform (gel type II), and lighter (with a force F at 15% less)than gel containing 2.5 wt.% hyaluronic acid, the same, but a uniform degree of crosslinking (gel type III).

Thus, this example proves that the gel according to the present invention with heterogeneous binding to a high degree and, therefore, a long time in tissues in vivo can be easily extruded by means of devices such as a thin needle.

Examples to metacestode or therapeutic use

Proposed invention the gel has been successfully used for medicinal purposes due to its ability to separate, to substitute, to fill in or increase the amount of biological tissues. For example, a patient who suffered from unilateral atrophy of the vocal cords, under local anesthesia has carried out a deep vnutrisutochnoi injection of hyaluronic acid gel according to Example 4. Due to its viscoelastic properties specialist in the field of laryngology able to accurately carry out the injection and to improve its regulation. Subsequently, the observed recovery of the volume of the vocal cords, which could provide significant measurable improvement in voice settings. This improvement lasted from 6 to 18 months, while the use is not suggested in the invention of the gel resulted in a more rapid resorption, less than 3-9 months in the case of the gel according to Example 2 due to the collapse of the gel under biochemical and enzymatic effects, loss of volume of the vocal cords and the deterioration of voice parameters.

Also there are many applications in the cosmetic field. The patient with mesh scar on the upper part of the nose in the surgical treatment of basal cell carcinoma using a thin needle gauge 30G subcutaneously introduced a small amount of hyaluronic acid gel according to Example 4. The gel was distributed around the scar and accurately dose is ovali depending on fill voids, to obtain a smooth surface, uniform with surrounding tissues without scar.

After retouching 30 days was obtained masking effect of the scar, which lasted for 15 months after the procedure. In the case of the use is not suggested in the invention of the gel according to Example 3 was impeded the introduction of the gel, was limited to the masking effect of the scar and long-term correction of the surface of the scar. In contrast, in the case of the use is not suggested in the invention of the gel according to Example 1 was received by the masking effect of the scar, but a few months after retouching was resorption.

Finally, the proposed invention, the gel may also Supplement or replace body fluids. The patient, who suffered from osteoarthritis of the knee of the third degree on a scale Kellgren and Laurence, using a thin needle 18G introduced a single dose proposed in the invention of the gel according to Example 4. According to the patient noted a rapid decrease in pain on a visual pain scale and the effect that lasted from 6 to 12 months, while the use is not suggested in the invention unstitched gel required three injections once a week each for pain relief, which disappears within 3-6 months after the last injection.

1. A method of obtaining a dense cross-linked biologically compatible polymer gel, zakluchali the Xia is what does the stage at which:
begin stitching the quantity, of at least one biocompatible polymer of natural origin in the solution by adding a certain amount of cross-linking agent,
carry out the crosslinking reaction of the above mentioned amount of polymer,
enter the extension number of polymer with molecular weight of over 500,000 Da in solution, in which the reaction mixture is diluted to reduce the concentration of polymer in solution, and carry out the stitching and
stop the crosslinking reaction by removing the cross-linking agent.

2. The method according to claim 1, characterized in that the stage of start stapling is carried out in an alkaline medium.

3. The method according to claim 1, characterized in that the stage of start stapling is carried out in an acid medium.

4. The method according to claim 1, characterized in that at the stage of introduction of the incremental amount of polymer injected additional amount of the crosslinking agent.

5. The method according to claim 1, characterized in that the stage of termination of stitching is carried out by dialysis.

6. The method according to claim 1, characterized in that the polymers of natural origin are compounds selected from the group comprising hyaluronic acid, chondroitin sulfate, keratan, Kermanshah, heparin, heparansulfate, cellulose and its derivatives, alginates, xanthan gum, carrageenin, proteins or kleinhovia acid.

7. The method according to claim 1, characterized in that at least one polymer of natural origin is a polymer, which by nature is not human organism selected from the group comprising cellulose and its derivatives, alginates, xanthan gum, carrageenin, a polymer made of at least one polymer, which by nature is present in the human body selected from the group comprising hyaluronic acid, chondroitin sulfate, keratan, Kermanshah, heparin, heparansulfate, proteins or nucleic acids.

8. The method according to claim 1, characterized in that the crosslinking agent is a two - or multi-functional molecule selected from compounds of the group, including epoxides, epichlohydrin and diphenylsulfone.

9. The gel obtained by the method according to claim 1.

10. The gel according to claim 9, characterized in that it is a gel containing at least one active principle dispersed.

11. Application of the gel according to claim 9 or 10 for separation, replacement or filling of biological tissue or to increase the amount of this fabric, or additions to, or replacement of biological fluid.



 

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10 cl, 8 tbl, 30 ex

FIELD: chemistry.

SUBSTANCE: method for preparation of functionalised, bound or star-block copolymer used in sulphur-cured rubber composition containing carbon char and having in cured state decreased hysteresis with at least one of said blocks containing polyisoprene and at least one other block consisting of diene elastomer different from polyisopren with mole content of repeating units of one or more of conjugated dienes exceeding 15% includes: copolymerisation of one or more monomers containing at least one conjugated diene different from polyisoprene with catalitycal system containing hydrocarbon solvent halogenated or unhalogenated metal-organic compound A of the group IIIA metal, alkaline-earth metal compound B and polymer initiator C containing bound C-Li formed by unfunctionalised monolythium-containing polyisopren intended for formation of the said block or every polyisoprene block and (ii) adding to the product of the said polymerisation of the functionalising, binding or star-shape forming agent containing acetoxy group of formula Rn-Sn-(O-CO-R')4n> whereat n is integer natural number from 0 to 4 and R and R' each represents following groups: alkyl, cycloalkyl, aryl, aralkyl, same or different, for functionalisation or binding or forming of star-shape structure of the said block consisting of dien elastomer different from polyisopren. The said one or more polyisopren blocks have number average molecular mass Mn1 from 2500 to 20000 g/mole, the said one or more dien elastomer blocks have number average molecular mass Mn2 from 65000 to 350000 g/mole. Functionalised, bound or star-block copolymer, curable or cured rubber composition with lowered hysteresis in cured state, containing reinforcing filler completely or partially consisting of carbon char and containing aforementioned functionalised, bound or star-block copolymer are described also. Pneumatic tyre tread containing aforementioned rubber composition is described as well as pneumatic tyre containing described above tread.

EFFECT: hysteresis decrease of cured the rubber composition.

36 cl, 5 ex

FIELD: mining.

SUBSTANCE: method for destructive treatment employed for intensified treatment of underground bed consists in preparing composition of viscous liquid on water base for treatment of bed; said composition contains water, polymer increasing viscosity and soluble in water composition for strongly retarded destruction of polymers containing source of hydrogen peroxide, source of ions of bivalent iron and chelating agent, wherein viscosity increasing polymer corresponds to polysaccharide; source of hydrogen peroxide is chosen from group consisting of tetra-hydrate of sodium perborate and hydrogen peroxide; soluble in water composition for strongly retarded destruction of polymers has molar ratio of chelating agent to source of ions of bivalent iron within range of from 3:1 to 6:1 and pH within range of from approximately 3 to approximately 7; further method consists in introducing composition of viscous liquid for bed treatment into underground section via borehole of well penetrating into underground section; also composition for strongly retarded destruction of polymer destroys composition of viscous liquid for bed treatment creating diluted liquid with low viscosity.

EFFECT: increased efficiency of underground bed treatment.

31 cl, 4 tbl

FIELD: chemistry, medicine.

SUBSTANCE: complex matrix consists of at least one biologically compatible polymer of natural origin, structured with sewing agent, which represents two- or multi-functional molecule, selected from epoxides, epihalohydrines and divinyl sulphone, on said polymer inoculated are chains with molecular weight less than 50000 daltons, selected from polymers of natural origin of small size, preferably, derivatives of cellulose or other biological polymer derivatives which naturally are not present in human organism, and/or non-polymerised chains with properties of oxidation inhibitors or ability to inhibit reactions of matrix decomposition, preferably, vitamins, enzymes or molecules, consisting of one or several cycles, degree of inoculation, expressed as ratio of moles of inoculated molecules and quantity of moles of polymer units, constitutes from 10 to 40%. Also described are method of obtaining such matrix and its application for separation, replacement, filling or addition of biological fluid or tissues.

EFFECT: increase of application efficiency.

20 cl, 7 ex, 2 tbl, 1 dwg

FIELD: chemistry, medicine.

SUBSTANCE: complex matrix consists of at least one biologically compatible polymer of natural origin, structured with sewing agent, which represents two- or multi-functional molecule, selected from epoxides, epihalohydrines and divinyl sulphone, on said polymer inoculated are chains with molecular weight less than 50000 daltons, selected from polymers of natural origin of small size, preferably, derivatives of cellulose or other biological polymer derivatives which naturally are not present in human organism, and/or non-polymerised chains with properties of oxidation inhibitors or ability to inhibit reactions of matrix decomposition, preferably, vitamins, enzymes or molecules, consisting of one or several cycles, degree of inoculation, expressed as ratio of moles of inoculated molecules and quantity of moles of polymer units, constitutes from 10 to 40%. Also described are method of obtaining such matrix and its application for separation, replacement, filling or addition of biological fluid or tissues.

EFFECT: increase of application efficiency.

20 cl, 7 ex, 2 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: present invention relates to the method of producing functionalised, linked or star block copolymer, used in rubber compositions, cross-linked with sulphur and with low hysteresis in the cross-linked state. Described is a method of producing the said copolymer, containing soot and with low hysteresis in the cross-linked state. At least one or the above mentioned blocks consists of a diene elastomer, distinct from polyisoprene, the molar content of branches of one or several conjugate dienes of which exceeds 15%. The method is distinguished by that it involves: (i) copolymerisation of one or several monomers, containing at least one conjugated diene, distinct from isoprene, using a catalyst system, containing a hydrocarbon solvent, halogenation or non-halogenated organo-metal compound A of a group IIIA metal, compound B of an alkali-earth metal and a polymer initiator C, containing C-Li bond, which is formed from non-functionalised mono-lithium containing polyisoprene, meant for forming the said or each polyisoprene block; the said one or several polyisoprene blocks have average molecular mass Mn1 from 2500 to 20000 g/mol, in effect that, one or several blocks, containing diene elastomer, distinct from polyisoprene, contains 70% or more 1,4-trans-branches and has average molecular mass Mn2 from 65000 to 350000 g/mol, and (ii) addition into the copolymerisation product of a functionalised, linking or star structure forming agent, containing one, two or at least three epoxy groups, respectively, for functionalising, linking or forming a star structure of the given block, consisting of diene elastomer, distinct from polyisoprene. Description is also given a functionalised, linked or star block-copolymer, cross-linkable or cross-linked rubber composition, containing the said functionalised, linked or star block-copolymer, and description is also given of a pneumatic tyre tread and a pneumatic tyre.

EFFECT: obtaining a block-copolymer, which is used in compositions for pneumatic tyre treads, and which reduces hysteresis of the given composition in cross-linked state.

40 cl, 4 ex

FIELD: chemistry.

SUBSTANCE: invention refers to making a moulded product for handling clean-room materials, intermediate products or end products, such as a container, a tray and a tool. The moulded product is made of resin compound prepared by mixing in melt cycloolefine polymer (A) 100 weight fractions chosen from the group including bicyclo[2.2.1]-2-heptene and its derivatives, tricyclo [4,3,0,12,5]-3-decene and its derivatives, and tetracyclo[4,4,0,12,5,17,10]-3-dodecene and its derivatives of vitrification temperature within 60 to 200°C, and amorphous or low-crystalline elastic copolymer (B(b1)) 1 to 150 weight fractions. Copolymer (B(b1)) is polymerised from at least two monomers chosen from the group including ethylene and a-olefin with 3 to 20 carbon atoms and vitrification temperature 0°C or lower. The compound contains radical polymerisation initiator 0.001 to 1 weight fractions containing peroxide, and polyfunctional compound (D) 0 to 1 weight fractions. The compound (D) has at least two radical-polymerised functional groups chosen from the group including vinyl group, allylic group, acrylic group and methacrylic group in a molecule.

EFFECT: clean-room moulded product is characterised with good chemical stability, heat resistance and dimensional accuracy, it prevents volatile component release in the surrounding space, has good abrasion resistance and prevents particle formation.

19 cl, 1 tbl, 2 dwg, 12 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing thermoplastic elastomer compositions, realised through dynamic vulcanisation of a mixture of components of a composition, meant for preparing sealing components, tubing, insulation for components of electric devices, used in aviation, automobile, cable and other industries. The method is realised by loading an ethylene-propylene-diene copolymer and target additives at the first step. Temperature is raised to 120°C and vulcanising agents are added. At temperature of 150°C, thermoplastics are added - polyethylene and polypropylene in amount of 30-50 wt % of their total content and stirring is done at temperature of 190°C. At the second step the remaining amount of thermoplastics is added to the obtained mixture.

EFFECT: obtaining a thermoplastic elastomer composition with improved mechanical, rheological and electrical characteristics.

3 cl, 1 tbl, 3 ex

FIELD: process engineering.

SUBSTANCE: proposed method relates to production of rubber-containing products, namely, to methods designed to control vulcanisation. Proposed method consists in correcting vulcanisation time depending upon that required for producing maximum modulus of rubber mix shear in vulcanising the specimens at flow metre and departure of rubber extension modulus in finished products from preset magnitudes. This allows processing disturbing effects on vulcanisation in compliance with tuber mix production and vulcanisation.

EFFECT: higher stability of mechanical characteristics of rubber-containing products.

5 dwg

FIELD: chemistry.

SUBSTANCE: description is given of a method of obtaining a fluoropolymer, containing nitrile terminal groups. The method involves free radical polymerisation of one or more fluorinated monomers in the presence of a salt, containing a nitrile group, or a pseudo-halogen compound, containing a nitrile group. Description is also given of a method of obtaining a fluoro-elastomer composition, a method of obtaining fluoro-elastomer and a solid fluoro-elastomer, containing nitrile groups at both ends, with formula: NCX-(Rf)-XCN, where X=O or S, and Rf is a bivalent fluoro-elastomer chain.

EFFECT: design of an efficient method of obtaining a fluoro-elastomer, containing nitrile terminal groups.

11 cl, 6 ex

FIELD: chemistry.

SUBSTANCE: thermoplastic elastomeric composition contains polypropylene, polyethylene, triple ethylene-propylene-diene copolymer, sulfur, primary and secondary vulcanisation accelerators, stearic acid and zinc oxide. Rubber crumb and bitumen are introduced into composition additionally. Combination of components in definite ratio improves rheological properties of composition and, correspondingly its processability.

EFFECT: high-strength products, of high ozone and atmosphere stability, resistance, can be practically fully utilised after expiry of product life.

5 cl, 2 tbl, 6 ex

FIELD: technological processes.

SUBSTANCE: rubber-polymer plates are designed for lining of different surfaces and structures exposed to permanent load and wear. Layer of uncured rubber 1.5÷20.0 mm thick is placed in mould with regulated shear deformation, above which layer of ultrahigh molecular polyethylene is evenly filled with molecular mass of 1.5·106 g/mole ÷ 10.0·106 g/mole. Volume of ultrahigh molecular polyethylene layer filling is calculated on the basis of final height of compact polyethylene layer, selected from 1.5 to 20.0 mm, cross section of mould and density of ultrahigh molecular polyethylene of 0.936 g/cm3. Then prepared composite is exposed to volumetrical compression in mould and then sintered at the temperature of 160÷210°C, pressure of 30 kg/cm2, and cure for 15 minutes - 1.5 hour.

EFFECT: preset thickness of plates and high strength of connection between layers.

FIELD: rubber technology.

SUBSTANCE: method is characterised by that, a sample is prepared for analysis during the vulcanisation process, for which 25 cm3 of toluene is added to a precise batch of the sample, with subsequent keeping the rubber mixture-toluene for 4 hours, after which gel-sol analysis is carried out. To carry out gel-sol analysis, the obtained system is filtered. The residue is dried until a constant mass is obtained. The content of gel in the system and concentration of polymer in the filtrate is calculated and its characteristic viscosity is determined. A graph is drawn with coordinates of characteristic viscosity - vulcanisation time and gel content - vulcanisation time, and from the character of the obtained graphic dependence the parameters of the vulcanisation process are determined. Two regions on the graph of the relationship between the characteristic viscosity of solutions and vulcanisation time are marked. On the first region, characteristic viscosity increases during the vulcanisation time of the sample in an almost linear relationship. In this case, the system contains gel, which shows that, in this period there not enough intermolecular transverse bonds in the sample to form a spatial structure, while the increase in characteristic viscosity is only a result of change in the length of caoutchouc macromolecules. The beginning of the vulcanisation process is shown by the increase in the characteristic viscosity of the investigated solution by 5% relative its minimum value. Content of gel increases from 0 to 100% in the second region. At the point with 90% gel content the sample is completely insoluble in toluene.

EFFECT: increased accuracy and efficiency of determining vulcanisation parameters on the initial stage of the process.

3 dwg

FIELD: chemistry.

SUBSTANCE: invention pertains to compositions of ternary copolymers on an isobutylene base and can be used in tyres, in particular in motor car components, such as protectors, inner lining of tyres, air bladders and tubes. The vulcanised elastomer composition contains halogenated ternary copolymer links from C4 to C8 derived from iso-olefin, links from C4 to C14 derived from multi-olefin and links derived from p-alkylstyrol. The composition is vulcanised in the presence of a sulphur vulcanising group. The value of adhesion to butadiene-styrene rubber of the vulcanising composition at 100°C is more than 70 N/mm. The composition also optionally contains filler and/or extra rubber. The suitable fillers are modified carbon black, carbon black, silicon dioxide, aluminium oxide, calcium carbonate, clay, mica, talc, titanium dioxide, starch, wood powder and their combination.

EFFECT: improved adhesion to the frame, elasticity with retention of impermeability to air.

52 cl, 1 dwg, 8 tbl

FIELD: rubber industry.

SUBSTANCE: method comprises mixing sulfur, zinc oxide, stearic acid, tetramethylthiuram disulfide, mercaptobenzothiazole, and carbon black. During the mixing process, a modifier is incorporated, said modifier having been preliminarily prepared via interaction, at 150°C, of 1.66-3.34 wt parts epoxide dian resin "ED-20" and 0.83-1.67 wt parts aniline production bottom waste containing 15-18 wt parts aniline at weight ratio of components 2:1, respectively.

EFFECT: improved physico-mechanical characteristics of rubber and increased adhesion thereof to metal when using chloroprene glues.

5 tbl

FIELD: rubber industry; other industries; compositions for production of the treads of the pneumatic tires and the methods of the compositions production.

SUBSTANCE: the invention is pertaining to the cross-linkable or cross-linked rubber composition characterized by the diminished hysteresis properties in the cross-linked state and by the improved manufacturability in the non-cross-linked state, to the method of its production, to the tread of the pneumatic tire and to the pneumatic tire. The composition contains the reinforcing filler consisting of the reinforcing inorganic filler, and, at least, one diene elastomer. The diene elastomer is produced in the form of the emulsion or the solution. The elastomer produced in the form of the solution has the molar contents of the conjugated dienes links exceeding 30 % and is produced at the following stages. At the first stage the initial diene elastomer is subjected to the reaction of the hydroaluminization or carboaluminization along the chain in the inert hydrocarbon solvent by addition to it of the aluminum-containing agent. At the second stage the produced product is added with, at least, one electron-seeking reagent intended for interaction with the indicated aluminum-containing agent. At the third stage they stop the process of the reaction of the second stage and extract the elastomer containing the functional groups of the carboxylic acid along the chain. The reinforcing inorganic filler is selected from the group including the highly dispersive silica, argil, Al(OH)3. The method of production of the composition includes the first stage of the thermomechanical treatment of the above-indicated elastomer and the reinforcing inorganic filler at the maximal temperature from 130°С up to 200°С, and the second stage of the mechanical working at the temperature smaller than the temperature of realization of the first stage with introduction of the cross-linking system. The diene elastomer received in the emulsion contains the functional groups of the carboxylic acid along the chain and is produced using the emulsifying solution by the method of the copolymerization by the following way. To the indicated emulsifying solution of the monomer or the monomers of the conjugated diene (the conjugated dienes) possibly with one or the several vinyl aromatic compounds add the comonomer consisting of unsaturated aliphatic carboxylic acid taken from the group consisting of the acrylic acid, the methacrylic acid, the maleinic acid, the fumaric acid. The method of production of the above-indicated composition includes the first stage of the thermomechanical working of an above-stated elastomer and the reinforcing inorganic filler, except for the system of cross-linkage at the maximal temperature from 130°С up to 200°С, and the second stage of the mechanical working at the temperature smaller than the temperature of realization of the indicated first stage with addition of the cross-linkage system. In one of the versions of the method the composition includes two phases of the first stage: At the first phase of thermomechanical working they introduce completely the whole amount of the monoxide for activation of the subsequent cross-linkage and intermix all the components, at the second phase they introduce the antioxidant and admix with components of the first phase. In the other version at the first phase of the first stage they introduce zinc monoxide and magnesium monoxide. The invention allows to produce the composition with the improved hysteresis properties in the cross-linking state and the pneumatic tire containing the tread produced from the composition with the reduced resistance to the rolling movement.

EFFECT: the invention ensures production of the composition with the improved hysteresis properties in the cross-linking state and the pneumatic tire containing the tread produced from the composition with the reduced resistance to the rolling movement.

20 cl, 10 tbl, 9 ex

FIELD: organic chemistry, polymers, chemical technology.

SUBSTANCE: invention relates to a composition used for cross-linking and stabilizing a polymer containing hydrolysable silane groups wherein this composition comprises sulfonic acid as a catalyst for condensation of silanols. Invention describes using the composition comprising sulfonic acid as a catalyst for condensation of silanols wherein sulfonic acid represents a compound of the formula (III): ArSO3H (III) or its precursor wherein Ar means hydrocarbyl-substituted aryl group, and compound comprises in total from 14 to 28 carbon atoms and wherein a compound used as a stabilizing agent represents neutral or acidic compound, it doesn't comprise ester groups and represents compound described by the formula (I):

wherein R means unsubstituted or substituted aliphatic or aromatic hydrocarbyl radical that can comprise heteroatoms; R' means hydrocarbyl radical; R'' means hydrocarbyl radical, and R' and/or R'' mean a bulky radical; X1, X2 and X3 are similar or different and represent hydrogen atom (H) of hydroxyl group (-OH) wherein at least X1, X2 or X3 mean -OH; n is in the range from 1 to 4. The composition is used for cross-linking and stabilizing a polymer comprising hydrolysable silane groups. Invention provides enhancing resistance of polymer against aging, absence of mercaptan or other odor and formation of cracks in material.

EFFECT: valuable properties of composition.

24 cl, 4 tbl

FIELD: chemistry.

SUBSTANCE: thermoplastic gel composition which can be cured under the action of radiation includes: (a) approximately from 5 to 40 wt % of cured block-copolymer selected from the group consisting from compounds of formula (II) or (III) or (IV), whereat A is vinyl aromatic hydrocarbon block with molecular mass from 4000 to 30000, HD is hydrogenated conjugated diene block with molecular mass from 10000 to 100000, Y is multifunctional binding agent, UD is conjugated diene block with molecular mass from 1000 to 80000 or conjugated diene block with molecular mass from 1000 to 80000 which is partially hydrogenated, x is integer number from 1 to 20, y is equal to 0 or 1, z is integer number from 1 to 20 and in the formulas (II) and (III) the sum (x+z) is in the range from 2 to 30; (b) from 60 to 90 wt % of the liquid component selected from the filling oils, plasticisers and solvents compatible with the curable copolymer; (c) from 1 to 20 wt % at least one curative agent selected from bifunctional or multifunctional acrylate or metaacrylate monomers or vinyl ethers; d) optionally from 0 to 10 wt % of the expanding microspheres; and (e) optionally from 0 to 3 wt % of the photoinitiator whereat total component amount is equal 100 wt %. The thermoreactive article containing the thermoplastic gel composition subjected to the action of radiation is described as well as the thermoplastic gel composition which can be cured under the action of radiation and includes: (a) from 5 to 40 % w/w of the mixture of curable block-copolymer with formula (I) whereat S is polystyrol block, B is polybutadiene polymer block having the content of 1,2-vinyl groups in the range from 10 to 80 mole %, Y is the radical of the binding agent, x is integer number from 1 to 20, preferably 2, y - integer number from 0 to 20, preferably 2, with sum (x+y) being in the range from 2 to 30; and block-copolymer of the (polystyrol -hydrogenated polybutadiene -polystyrol ) type with ratio (block-copolymer of formula (I): (block-copolymer of (polystyrol -hydrogenated polybutadiene -polystyrol ) type being in the range from 3:1 to 1:3; (b) from 60 to 90 wt % of the liquid component selected from the filling oils, plasticisers and solvents compatible with the curable copolymer; (c) from 1 to 20 wt % of at least one curative agent selected from bifunctional or multifunctional acrylate or metaacrylate monomers or vinyl ethers; (d) from 0.1 to 10 wt % of expanding microspheres; and (e) from 0 to 3 wt % of photoinitiator whereat total component amount is equal 100 wt %.

EFFECT: increase of high-temperature shrinkage resistance.

10 cl, 8 tbl, 30 ex

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