Method of producing oligodimethylsiloxanes. RU patent 2513022.
 Kieselsol material with, at least, one therapeutically active substance for obtaining biologically decomposable and/or absorbable kieselgel materials for medicine of people and/or medical equipment / 2512512Invention relates to novel kieselsol material with, at least, one therapeutically active substance for obtaining biologically decomposable and absorbable kieselgel materials. Claimed is kieselsol material with, at least, one therapeutically active substance, obtained by reaction of hydrolysis-condensation of tetraethoxysilane, catalysed by acids with initial pH value from 0 to ≤7 in presence of water-soluble solvent for at least 16 hours at temperature 0-80°C; with further evaporation with obtaining one-phase solution; cooling obtained solution with further maturation at temperature 2-4°C with formation of homogeneous one-phase sol. Addition of local anesthetic is performed at one of the described stages. Also claimed are versions of applying said kieselsol material and obtained from it biologically absorbable or bioactive powder, monolith or coating and biologically decomposable or biologically absorbable fibrous material. |
 Nontoxic polysiloxane material for making articles containing biodegradable and/or bioactive polysiloxane material, production and use thereof / 2496804Invention relates to nontoxic polysiloxane material. Disclosed is biodegradable polysiloxane material for making fibre by (a) a first hydrolysis-condensation reaction of at most residue of one or more different Si compounds of formula SiX4, where residues X are identical or different, the reaction being catalysed by acid agents and at initial pH from 0 to ≤ 7, in the presence of a water-soluble solvent for 1-192 hours at temperature of 0-80°C, (b) a second hydrolysis-condensation reaction of material obtained at step (a), conducted with simultaneous removal of solvent by evaporation in a closed mixing apparatus while continuously feeding a chemically inert stream of a carrier gas in a vacuum of 1-1013 mbar at temperature of 30-90°C to viscosity of 0.5-2 Pa∙s. At step (c) the polysiloxane material is cooled in a closed apparatus to temperature of -20 - +10°C for 2 min to 5 hours, and then (d) the polysiloxane material obtained at step (c), via a third hydrolysis-condensation reaction, is converted to matured polysiloxane material at temperature of -20 - +10°C for 1 day to 8 weeks, wherein step (d) is carried out immediately after step (c). |
 Method of producing siloxane rubber modified with diphenyl units / 2487143Disclosed is a method of producing siloxane rubber modified with diphenyl units via co-condensation of diphenylsilanediol with a prepolymer which is obtained by copolymerisation of dimethylcyclosiloxanes and methylvinylcyclosiloxanes in the presence of an anionic catalyst, wherein the co-condensation reaction is carried out in the presence of an additional portion of said anionic catalyst at temperature of 130-170°C with azeotropic distillation of water and subsequent neutralisation of the anionic catalyst and distillation in a vacuum of unconverted cyclosiloxanes. |
 Method of producing α,ω-bis(methyl diphenylsilyl)-oligodiorganosiloxanes / 2471818Invention relates to methods of producing oligodiorganosiloxanes, used as working fluid in oil-vapour vacuum pumps for creating moderate and ultrahigh vacuum; as working medium for droplet cooler-radiators of frameless systems for removal of low-grade heat of space nuclear power systems. Disclosed is a method of producing α, ω-bis(methyl diphenylsilyl)oligodiorganosiloxanes of formula (I), where k=1,2; for k=1 R=Me (1a), R=Ph (1b); for k=2 R-Ph (1c), by condensation of diorganodichlorosilane and sodium methyl diphenyl silanolate, involving a step for drying the sodium methyl diphenyl silanolate, which is carried out using dimethyl dichlorosilane which is taken in amount of 0.1-1 mol % of the amount of sodium silanolate. |
| Method producing coating material / 2468042 Invention relates to a method of producing coating material. Disclosed is a method of producing coating material in form of powdered lacquer or a fluid resin, characterised by that one or more alcohols or polyols react with one or more silanes selected from a group consisting of (isocyanatomethyl)methyl-dimethoxysilane, 3-isocyanatopropyl-trimethoxysilane and 3-isocyanatopropyl-triethoxysilane, to form a covalent bond between the alcohol or polyol and the silane such that the reaction product is a high-molecular weight silane which is cured directly using a catalyst, wherein all alcohol or polyol organic functional groups participate in the reaction with the silane organic functional group. Coating material and use thereof are also disclosed. |
| Method of producing heat-resistant oligoorganosiloxane resins / 2464286 Invention relates to the technology of producing oligoorganosiloxane resins used in production of composite materials for different purposes, as a film-forming component of lacquer when producing protective coatings and for modifying organic lacquer and resins. Disclosed is a method of producing heat-resistant oligoorganosiloxane resins of formula [PhSiO3/2]a[RnSiO1.5]b[Me2SiO]c, where Rn - Me, H, Vin, where n=1; a=0.5-0.97; b=0.03-0.5; c=0-0.47 by polycondensation of products of hydrolysis starting organoalkoxysilanes in an active medium which is an anhydrous carboxylic acid under the effect of a catalyst which is sulphuric acid, characterised by that the mixture of starting organoalkoxysilanes, selected from PhSi(OEt)3, RnSi(OEt)4-n, where Rn=Me, H, Vin, where n=1, first undergoes partial hydrolysis at temperature 70°C, where the catalyst - sulphuric acid - is taken in amount of 0.001-0.09 mol % of the total number of moles of starting organoalkoxysilanes, and to improve elasticity of the obtained product, cyclosiloxane [Me2SiO]4 which does not contain chlorine is added to the mixture of starting organoalkoxysilanes. |
| Method of producing polyorganosiloxanes / 2463319 Disclosed is a method of producing polyorganosiloxanes by reacting α,ω-dihydroxy dialkyloligosiloxane with dialkyl-bis-(N,N-dialkylamino)silanes at room temperature in an atmosphere of an inert gas for 1-10 hours in the presence of an alkylamide of a carboxylic acid. |
 Phenoxyethanol oligoethoxysiloxane derivatives for modifying fibre materials and production method thereof / 2456309Disclosed are phenoxyethanol oligoethoxysiloxane derivatives of structural formulae (I) and (II) Disclosed also is a method of producing the disclosed compounds by heating a mixture of oligoethoxysiloxane and phenoxyethanol to 80°C, holding at that temperature with slow distillation of the formed ethanol and subsequent cooling of the residue to room temperature. |
 Method of producing linear polydimethylsiloxanes with terminal hydroxyl groups via polycondensation of dimethyldialkoxysilanes in active medium / 2456308Disclosed is a method of producing linear polydimethylsiloxanes with terminal hydroxyl groups, involving polycondensation of dimethyldialkoxysilane selected from dimethyldialkoxysilanes of general formula (CH3)2Si(OAlk)2 (I), where Alk denotes an alkyl group from C1 to C4, wherein the polycondensation process is carried out in an active medium which is an anhydrous carboxylic acid selected from: formic, acetic, propionic, isobutyric, trimethylacetic acid, with subsequent removal of volatile components. Molar ratio of dimethyldialkoxysilane to carboxylic acid ranges from 1:3 to 1:10. The polycondensation process in the active medium is carried out at temperature ranging from 20°C to boiling point of the reaction mixture, and removal of volatile components is carried out in a vacuum at temperature ranging from 20°C to 150°C. Depending on conditions for polycondensation of the initial dimethyldialkoxysilane, molecular weight of the reaction product ranges from 3500 to 70000. |
 Method of producing linear polymethylphenylsiloxane with terminal hydroxyl groups via polycondensation of methylphenyldialkoxysilane in active medium / 2456307Disclosed is a method of producing linear oligomethylphenylsiloxanes with terminal hydroxyl groups via polycondensation of methylphenyldialkoxysilane selected from methylphenyldialkoxysilanes of general formula (I) (CH3)(C6H5)Si(OAlk)2 (I) where Alk denotes an alkyl group from C1 to C4, in an active medium which is an anhydrous carboxylic acid until complete conversion of alkoxy groups. The carboxylic acid used is selected from: formic, acetic, propionic, isobutyric and trimethylacetic acid. Molar ratio of methylphenyldialkoxysilane to carboxylic acid ranges from 1:3 to 1:10. The polycondensation process in the active medium is carried out at temperature ranging from 20°C to boiling point of the reaction mixture. Removal of volatile components is carried out in a vacuum at 20°C. |
 Method for production of siloxane oligomers / 2285017Described is method for production of siloxane oligomers of general formula I or II , wherein oligomer has at least one functionalized alkyl group in molecule. Claimed method includes oligomerization of haloalkyltrihalosilanes in presence of alcohol and water and optionally cooligomerization with C1-C18-alkyl-, phenyl, aryl- or alkyltrihalosilanes and/or silicium tetrachloride; and in the further step haloalkyl functionality is optionally modified. |
 Continuous process for production of dimethyldichlorosilane hydrolyzate / 2315781Invention relates to acid hydrolysis-mediated production of dimethyldichlorosilane hydrolyzate, which is useful in manufacture of low molecular weight siloxane rubbers, polymethylsiloxane liquids, compounds, and other polymer materials. Invention is directed to provide continuous process for production of dimethyldichlorosilane hydrolyzate enabling achievement of stable high qualitative characteristics of desired products. Proposed continuous process comprises hydrolysis of dimethyldichlorosilane performed by direct-counter mixing of dimethyldichlorosilane with concentrated hydrochloric acid at pulse ratio I=50-250, separation of liquid into acidic hydrolyzate and concentrated hydrochloric acid in force field at accelerations α=1.0-5.0 g, recycling of acid to hydrolysis stage, after-hydrolysis of acidic hydrolyzate with hydrochloric acid in extraction mode at 50-70°C to form hydrolyzate and 10-20% HCl (which is returned to hydrolysis stage), washing of hydrolyzate with water at 70-90°C, and separation of water from hydrolyzate by passing the latter through coalescenting material followed by settling. |
| Method for preparing polyphenylethoxysiloxane / 2320678 Invention relates to method of synthesis of polyphenylethoxysiloxanes that are used broadly for modification of organic lacquers and resins, and as binding agents in production of refractory insulating materials. Invention proposes a method comprising the hydrolytic esterification reaction of phenyltrichlorosilane under atmosphere pressure with aqueous-alcoholic mixture containing 10-12 wt.-% of water, in the mole ratio of reagents phenyltrichlorosilane : water : ethyl alcohol = 1:(0.7-0.8):(2.2-2.7), respectively, at temperature 20-30°C and with simultaneous removing evolving hydrogen chloride and the following vacuum desorption of hydrogen chloride from the reaction mass up to the concentration of residual chlorine 0.04%, not above. The ready solvent-free product doesn't require additional purification and neutralization. Invention provides creature the method providing preparing stable solvent-free polyphenylethoxysiloxane. |
 Method of obtaining polyorganosiloxanes / 2346960Invention concerns synthesis of high-molecular organosiloxanes and claims method of obtaining organosilicon fluids of the formula I by exposing organocyclotrisiloxane mix at 50-120°C to the effect of sodium hydroxide or siloxanediolate catalyst in amount of 0.004 to 0.1 wt % rated against added alkali, in the presence of acetone activation agent in amount of up to 0.15 wt % and water in amount of 0.005-2.0 wt % in inert gas environment under pressure of 1-2 atmospheres. Catalyst is neutralised at (20-25)°C by carbon dioxide under pressure of 2 to 4 atmospheres. Method allows obtaining polyorganosiloxanes of various composition and wide range of molecular weight, applicable as a basis for damping fluids, rubbers, seals, coatings etc. where: R=CH3-; R'=C6H5-, CF3CH2CH2-; R"=CH2=CH-; k=1-1500; 1=1-2000; m=0,1-3; n=3-500. |
 Polyorganoacetoxysiloxane process / 2357978There is disclosed polyorganoacetoxysiloxane process with terminal acetoxygroups characterised by 4-64 organosilxane links in polymer, involving reaction of acetoxy- and organosiloxanes with alkylcyclotri-, -tetra-, -penta- and hexasiloxanes or their mixture in molar component ratio 1:(1-16) respectively. The reaction product is heated to 70-100°C with a catalyst represented with mixed sulphuric and acetic acids. Upon completion of reaction, sulphuric acid is neutralised with sodium acetate to separate an end product of yield 83-93 wt %. Owing to high adhesion of polymers, the products are used as cross-linking agents for hardening of various compounds, and as sealants and heavy duty revetments. |
 Method of producing organosilicon resins / 2384591Method is proposed for producing organosilicon resins containing silicon dioxide structural fragments, in which the initial components used are hexaorganodisiloxane of general formula [R'R2Si]2O, where R=-CH3; R'=-CH3; -C6H5; -CH=CH2 or its mixture with organoalkoxysilanes of general formula RnSi(OR')4-n, where R'=-CH3; -C2H5; n=1, 2, 3 and a product of partial hydrolysis of tetraethoxysilane, acidolysis is carried out in the presence of catalytic amounts of trimethylchlorosilane with subsequent heating of the reaction mass until boiling and holding for 1-6 hours until formation of the end product. Proposed method excludes and considerably reduces use of aliphatic alcohol, reduces consumption of acetic acid and reduces formation of byproducts. Obtained resins can be used as modifiers of organosilicon and organic rubber and liquids, as well as binder components for making new generation polymer composite materials. |
 Oligo(alkylene)alkoxy siloxanes for modifying fibre materials and synthesis method thereof / 2387677Oligo(alkylene)alkoxy siloxanes of general formula are proposed, where R=CH3; C2H5; C3H7; C4H9; x=0,1; m=5-15, as well as a method for their synthesis through hydrolytic condensation of alkylene trialkoxy silane with given amount of water in a liquid alcohol-water medium while boiling. |
 Method for synthesis of aminooxyalkylene-containing oligoalkoxy siloxane and self-emulsifying composition based on said compound / 2389734Invention relates to methods for synthesis of organosilicon compounds which self-emulsify in water and compositions based on said compounds. A method is proposed for synthesis of aminooxyalkylene-containing oligoalkoxy siloxane (component A) through hydrolysis of a mixture of organotrialkoxysilanes and an oligoalkoxy siloxane-oligooxyalkylene block-copolymer with mass ratio of reagents equal to (1-9):(0.02-1) in the presence of a 20% HCl solution catalyst and co-condensation of the obtained semi-product with addition of amine-containing organotrialkoxysilanes with subsequent distillation of alcohol and neutralisation of the end reaction product. Proposed also is a self-emulsifying composition for porous construction materials, consisting of components A+B in ratio 1:(1-4), where B is organotrialkoxysilane used in the hydrolysis process as a reagent of the initial mixture. |
| Photopolymerisable organosilicon composition for gluing and sealing optical elements and method of preparing base for said composition / 2393195 Invention relates to photopolymerisable adhesive compositions for gluing and sealing glass optical elements of different optical devices working on the border of visible and near UV band. The engineering problem lies in preparing a photopolymerisable organosilicon composition for gluing and sealing optical elements, which has high optical transmission in the wavelength range from 220 to 700 nm, has no intrinsic fluorescence and is distinguished by high versatility. A composition is disclosed, which has a base in form of a mixture of oligomers with general formula: R1Si(CH3)2O-[Si(CH3)2O]n-Si(CH3)2R2, where R1=OCH2CH(CH2Cl)-OCOC(CH3)=CH2, R2=OH, OCH2CH(CH2Cl)-OCO-C(CH3)=CH2, 1.5-2.0 radicals with double bonds in a molecule; n=50-300, and a photoinitiator selected from benzyldimethylketal, hydroxypropylacetophenon and 1-hydroxycyclohexylphenylketone, added in amount of 1.5-0.5 pts.wt per 100 pts.wt of the mixture of oligomers. Also disclosed is a single step method of preparing a mixture of oligomers (bases), characterised by that α,ω-dichloroligodimethylsiloxane is reacted with glycidyl methacrylate (GMA) in the presence of a dimethylformamide (DMFA) catalyst. |
 Method of producing organosilsequioxanes / 2414484Invention relates to a method of preparing a composition which contains organosilsequioxanes. Disclosed is a method of preparing a composition which contains organosilsequioxanes, comprising the following steps: (1) partial hydrolysis of hydrolysing inorganic monomer precursors which contain at least 50 mol % first hydrolysing inorganic monomer precursors of formula RSiY3, where R is selected from (cyclo)alkyl, aryl, alkenyl, epoxy-, (meth)acrylic, ester, amino-, mercapto- and cyanate groups and mixtures thereof, the R-Si bond is a non-hydrolysing bond, each Y group is identical or different from every other Y group of the alkoxy group; (2) cooling the liquid composition before completing condensation of inorganic monomers with an amount of water which, combined with water used at step (1), and any water separated during condensation of inorganic monomers at step (1), exceeds the stoichiometric amount of water needed for complete hydrolysis of all present precursors of hydrolysing inorganic monomers; and (3) drying the composition, wherein the total amount of water used is at least 5 times more than the stoichiometric amount of water needed for complete hydrolysis of all present hydrolysing monomer precursors. |
FIELD: chemistry.
SUBSTANCE: disclosed is a method of producing oligodimethylsiloxanes via rearrangement of dimethylcyclosiloxanes and/or a hydrolysate of dimethyldichlorosilane in the presence of hexamethylsiloxane and a catalyst - a sulphonated copolymer of styrene and divinyl benzene with content of the latter ranging from 25 wt % to 50 wt %, where the initial step of the process involves activating the catalyst by adding liquid polymethylsiloxane with viscosity of 10-50 cSt to the reaction mixture, wherein activation and production of oligodimethylsiloxanes are carried out in a current of inert gas with specific consumption of 0.2 m3/h per 1 kg catalyst in fluidisation conditions at temperature of 70-90°C.
EFFECT: high efficiency of the method by cutting duration of the induction effect as a result of catalyst activation and improved quality of the obtained oligodimethylsiloxanes by reducing the polydispersity index.
3 cl, 2 dwg, 4 ex
The proposed invention relates to methods of obtaining oligoaniline, namely to a method of obtaining oligomerisation, which are used as instrument of liquids, foundations greases, coolants, working liquids of different hydraulic systems, modifiers synthetic fibers, etc.
A method of obtaining of oligodimethylsiloxanes in which oligoethoxy get rearrangement at a temperature of 110-120 C in the mode of fluidization of salidroside mixture of amoksicillinom in the presence of catalyst - sulfonated styrene and divinylbenzene (A.S. USSR 887586, IPC C08G 77/06, 1981). Mode of fluidization in the system "gas-liquid-solid" provides high efficiency of the process of catalytic rearrangement due to the highly developed surface of contact of phases and intensive mass exchange at the interface "solid catalyst-liquid phase" through microturbulence diffusion.
The disadvantage of this method are high process temperature close to the temperature of decomposition catalyst that leads to its thermal degradation.
The closest to the technical substance and achieved the effect of the present invention, and taken as a prototype is a way to get oligoaniline by regrouping of hydrolysis product organochlorosilanes or their mixtures in the presence of sexualintimacy and catalyst, which is used sulphonated copolymer of styrene and divinylbenzene with the content of the last 25 to 50% weight. Catalytic regrouping carried out at a temperature 70-75°C with a tenfold use of the catalyst. (asscr 312855, IPC C08G 31/09, 1971).
The disadvantage of this method is to reduce the activity of the catalyst at its multiple use, which leads to the increase of time of process and, consequently, decrease performance. Intensification of the process by increasing the speed agitators in this case, as this is a mechanical grinding of the catalyst and its partial deactivation due to violation of the structure of the surface. Furthermore, the presence of fine-dispersed phase complicates the process of separation of the catalyst from the reaction product.
If the reaction in capacitive reactor mixer must also take into account the induction period in the work of the catalyst, when the efficiency is low, and take a certain margin of working volume of equipment, resulting in increased capital and operating costs for the production of oligoaniline.
Object of the present invention is to eliminate these shortcomings, improving the efficiency of the process of obtaining oligoaniline higher quality.
The problem is solved by the fact that the new method of obtaining oligomerisation, includes the rearrangement of dimethylcyclohexanes (DMCS) and/or hydrolysate clear (DMDS) in the presence of an agent of an open circuit - hexamethyldisiloxane (GMDSS) and catalyst - sulfonated styrene and divinylbenzene with the content of the last 25 to 50% of the mass., wherein for intensification of the initial stage of the process is conducted activation of the catalyst process by introducing in the reaction mixture polimetilsiloxan (PMS) liquids with viscosity 10-50 FTAs in the amount of 0,01-0,05 kg per 1 kg of the catalyst at 70-90°C, but the activation and receive oligomerisation are in the mode of fluidization using inert gas. As an inert gas can be used nitrogen with specific consumption of 0.2-2 m 3 /h on 1 kg of a catalyst.
The technical result consists in increasing the productivity by reducing the time of induction effect in the result of the activation of the catalyst and by maintaining a high-activity catalyst with repeated use (up to 15 times) in the mode of fluidization. In addition, oligomerisation obtained by the proposed method are of a higher quality due to decrease of the coefficient of polidispersity that affects their application properties.
According to the authors of this technical solution, low viscosity polimetilsiloxan (PMS) the liquid is introduced into the reaction mass on initial boot, dissolve, either physically removes (wash) with active centers of the catalyst surface some characteristic inherent in the method of catalyst production of chemical compounds, usually blocking these active centers. Activation of the catalyst PMS-liquid makes available and includes all of the active centers on the surface of the solid catalyst. Due to this treatment, process efficiency, as measured by changes in the viscosity of the reaction products is increasing, while remaining at a constant high level during the whole period of catalytic rearrangements. The induction period is significantly reduced or completely eliminated. In this case, to consider the induction period and do reserve the reaction volume equipment to provide power is required. The decrease in equipment, in turn, leads to the decrease of the volume of the reaction mass and reduction of the charge of inert gas that is required to ensure the regime of fluidization, so in addition to capital costs are also reduced and the operational costs of the process.
The method is as follows. In the vertical apparatus with the jacket for heating of the reaction mixture, consisting of two zones (cylindrical bottom of the reaction zone and the upper zone of the separator), equipped with temperature control devices on the grid, mounted in a cylindrical part of the device, download the operational quantity of the catalyst. In the lower area of the device pour reaction mixture containing dimethylcyclohexane and/or hydrolyzed clear, hexamethyldisiloxane and activator - polimetilsiloxan liquid (ICP-10). From the bottom of the device under a mesh catalyst serves nitrogen speeds ranging from 0.2 to 2.0 m 3 /h per 1 kg catalyst for a regime of fluidization in the system of gas-liquid-solid and heated reaction mass to the required temperature. The activation of the catalyst at 70-90°C with specific consumption activator 0,01-0,05 kg per 1 kg of the catalyst allows you to get the most effective result of activation of the catalyst.
The essence of the proposed technical solution is illustrated by the following examples.
Example # 1
Getting oligodimetilsiloksana viscosity 10 cSt (polimetilsiloxan fluid PMS 10) with the addition of the activator - polimetilsiloxan fluid viscosity 10 FTAs.
In the reactor column type with a shirt with a volume of 2 liters of load:
1300 g dimethylcyclohexane (DMCS), 600 g hexamethyldisiloxane (GMDSS); 98 g catalyst - sulfonated styrene and divinylbenzene, activator (ICP-10) - 2, Include the heating of the reactor and the supply of nitrogen consumption 0.02 m 3 /H. Further raise the temperature in the reactor up to 75 degrees C and every 20 min determine the viscosity of the liquid phase. When reaching viscosity 9-10 FTAs process to stop it.
Figure 1 shows a graph of the dependence of viscosity oligomerisation fluid from the time of synthesis, from which it follows that the viscosity is obtained oligomerisation liquid 9,4 FTAs is achieved 50 min (schedule №1).
Example 2 (comparative)
Getting fluids PMS-10 without the use of the activator.
In the reactor column type shirt with 2-liter download: DMZS - 1300 g; GMDSS - 600 g; catalyst - 98, Include the heating of the reactor and the supply of nitrogen. Nitrogen supplied to the bottom of the reactor with a flow rate of 0.02 m 3 /h Next, raise the temperature in the reactor up to 75 degrees C and every 20 min measure the viscosity of the liquid phase. When reaching viscosity 9-10 FTAs process to stop it.
The viscosity of the reaction mixture over time is shown in Fig1 (diagram №2).
Fig.1 shows that the viscosity of 9.5 FTAs achieved 95 min (diagram №2).
Example # 3
Getting oligoadenilatsintetaza with 400 cSt viscosity (polimetilsiloxan fluid PMS-400) using the activator.
In the reactor column type shirt with 2-liter download: hidrolizat MDHS - 1870; GMDSS - 30 g; catalyst - 98 g; activator (ICP-50) - 2,
Include the heating of the reactor and the supply of nitrogen. Nitrogen supplied to the bottom of the reactor with the consumption of 0.2 m 3 /H. increase the temperature in the reactor to 85 degrees C and every 20 min measure the viscosity of the liquid phase. When reaching viscosity 390-400 FTAs process to stop it.
The viscosity of the reaction mixture over time is shown in Fig.2 (schedule №1).
Figure 2 shows that the viscosity 390 FTAs achieved 110 min (schedule №1).
Example # 4 (comparative)
Getting fluids PMS-400 without the use of the activator.
In the reactor column type shirt with 2-liter download: dmdcs hydrolyzate - 1870; GMDS - 30 g; catalyst - 98,
Include the heating of the reactor and the supply of nitrogen. Nitrogen supplied to the bottom of the reactor with the consumption of 0.2 m 3 /H. Further raise the temperature in the reactor up to 90 degrees C and every 20 min measure the viscosity of the liquid phase. When reaching viscosity 390-400 FTAs process to stop it.
The viscosity of the reaction mixture over time is shown in Fig.№2 (diagram №2).
Figure 2 shows that the viscosity 390 FTAs achieved 160 min (diagram №2).
So, as you can see from the examples above, the proposed solution allows to increase efficiency of the process of obtaining oligomerisation.