Method for desalination of phenol resin and apparatus for realising said method

FIELD: chemistry.

SUBSTANCE: present invention relates to a method for desalination of phenol resin and apparatus to that end. The disclosed method involves mixing starting components - phenol resin, diisopropyl ether, water and concentrated sulphuric acid at temperature 20-60°C, phase separation of the mixture into a top organic layer, which is a mixture of desalinated phenol resin and ether, and a bottom aqueous layer with subsequent removal of the aqueous layer and distillation of ether from the organic layer and obtaining desalinated phenol resin, wherein the obtained ether is fed to the step for mixing components. The starting components are used in the following weight ratio: resin : ether : water : sulphuric acid = 1 : (0.2-0.6) : (0.7-1.0) : (0.007-0.018), wherein mixing is carried out in turbulent conditions.

EFFECT: present invention enables to obtain desalinated resin with high degree of purity while reducing the cost of the process and the obtained product.

13 cl, 24 ex, 6 tbl, 2 dwg

 

The group of inventions relates to the field of industrial organic synthesis, namely the processing and recycling of large co-production of phenol and acetone Kukolnik method Kruglova (Kruglov D., Golovenko B. I. - M.: Goskomizdat, 1963), in particular to the desalting phenolic resin.

Currently komorny the process of production of phenol and acetone as by the classical technology of single-stage or a modern two-stage decomposition process technical cumene hydroperoxide (intermediate product Kumanovo method) characterized by the formation of byproduct phenolic resin, the output of which is from 50 to 200 kg per ton of phenol.

Phenolic resin (the resin) is an oily viscous liquid with a characteristic pungent odor is a byproduct of the production of phenol and acetone is produced according to the technical requirements and standards for THE 2424-05757601-98 "phenolic Resin". The resin has at 20°C the density of 1.06-1.10 g/cm3and the refractive index of 1.57-1,59, melting point 42,9°C, boiling 181,9°C, flash 61°C and C 595°C. composed of phenolic resin contains up to 8% of the phenol in the form of phenolate sodium, acetophenone 10-15%, of α-methylstyrene to 1%, the dimers of α-methylstyrene 20-30%, isomers of cumylphenol 25-45%, dimethylphenylcarbinol to 7%, cumene to 1%, resinous what soedineniya and moisture, as well as mineral salts, including sodium sulfate, calculated on the sodium of 0.014÷0,034%. When the temperature drops to 0-5°C. the resin is prone to salustiano and crystallization, which is associated with the presence of cumylphenol. Phenolic resin is a high-calorie boiler fuel with calorific value 37254 kJ/kg.

Currently, the phenolic resin is illiquid commodity product. It is known that most of the methods of disposal and recycling of phenolic resins require prior purification of salts. Therefore, improving the quality phenolic resin by desalting would significantly expand the possibilities of rational way of recycling and waste - composition chemical modification of obtaining products for various industrial uses - phenol-formaldehyde resins, bitumen, etc. or when it is used as raw material in the production of technical carbon, coke, as well as boiler fuel. For example, in the production of technical carbon content of sodium ions in the phenolic resin should not exceed 0.01% wt. High content in phenolic resin of sodium ions of 0.014÷0,034% leads to the high ash content of 0.4÷0.8% and coking ability to 5% and dramatically affects the quality phenolic resin as boiler fuel. When the combustion temperature phenolic resin more 1430°C is then fusing into three ions is in the material of the furnace, which leads to lowering its melting temperature and melting or destruction, and the sodium sulfate is deposited in the furnace of the recovery boiler convective beams, pipes and heat exchangers that impedes heat transfer and causes the need for manual cleaning of the specified node.

Known methods of desalting phenolic resin 10%solution of sulfuric acid (Wills - Epstein. Refining and petrochemicals. - M.: Tsniiteneftehim, 1965, No. 10, p.37; A.S. USSR 139662). In this part present in the phenol resin salt, representing the reaction of sodium and iron, into salts of sulfuric acid and together with the main mass of sodium sulfate is transferred into an aqueous solution of sulfuric acid. The process is carried out at a temperature of 50-60°C. the Ratio of resin and solution of sulfuric acid is 1:0.5 to volume.

The disadvantages of the known technical solutions include the use of a large number of H2SO4a rise in the cost of the process; the emergence of a large number of industrial wastewater, contaminated products neutralize acids; increased corrosion of process equipment.

The closest in technical essence and the achieved effect of the claimed method is a method of desalting phenolic resin (Patent for inventions EN 2057110) by multistage extractive processing of phenolic resins in the Oh in the presence of solvent diisopropyl ether (the ether) or cumene at a mass ratio of resin:air:water = 1:0,9:0.6 or resin:cumene:water = 1:1,5:0.6mm. At the last stage desalting resin used steam condensate. In order to avoid the formation of stable emulsions pH of the working environment in the process of demineralization support no more than 7. The process of demineralization resin conduct multi-stage: 1st stage resin is mixed with the solvent; in the 2nd step the resulting mixture is mixed with water 2-stage extraction; 3-tier spend the stratification of the mixture of organic and aqueous layer; the 4-th stage of the organic layer (a mixture of resin and ether) are mixed with water 3-stage extraction and sulfuric acid; 5-tier spend a bundle on an organic and an aqueous layer; 6-tier mixed organic layer with steam condensate; on the 7th stage spend a bundle on an organic and an aqueous layer; at 8th level, conduct the distillation of the solvent from the organic layer and get desalted phenolic resin with a content of 0.003% by weight. sodium ions.

Closest to the claimed device is a device for desalting phenolic resin (Patent RU No. 2057110), including four of the mixing tank with agitator for mixing the components and three Florentine vessel for separating a mixture of components on the upper organic and lower water the layer, distillation column for distillation of the solvent to obtain a desalted phenolic resin.

Undoubted advantages and benefits of this method and demineralizing plant phenolic resins are providing more environmentally friendly technologies that reduce the consumption of such chemicals as sulfuric acid, sodium hydroxide, sodium carbonate, etc., reducing corrosion of equipment, the use of simpler and cheaper materials for its production.

Significant disadvantages of the known technical solutions include a mixture of phenolic resin with water without the addition of sulphuric acid on the 1st stage, which leads to the formation of 2-tier stand emulsion of phenolic resin and the complication phase separation of the organic and the aqueous layer was on the 3rd level; the use in the process of scarce steam condensate; used as a solvent cumene with a high boiling point; using in the process a large number of ether; process at high temperature 40-50°C; multi-stage or multi-stage, many recyclo water layer and the consumption of the process, the complexity and the complexity of its hardware design and, as a consequence, the large capital costs of industrial implementation.

Task group izobreteny which is the creation of more efficient technologies for desalination of phenolic resin to obtain desalted phenolic resins of high purity while reducing the cost of the process and resulting product.

The technical result is to reduce the time of carrying out the process of desalination of phenolic resins, including by reducing the time spent on mixing components and phase separation.

The problem is solved in that in the method of desalting phenolic resin comprising mixing the starting components - phenolic resins, diisopropyl ether, water and concentrated sulfuric acid at 20 to 60°C., phase separation of the mixture on top of the organic layer, which is a mixture of demineralized phenolic resin with ether, and the lower aqueous layer, followed by removal of the aqueous layer and distillation of the ether from the organic layer and obtaining desalinated phenolic resin, thus obtained ester is directed to the step of mixing the components according to the invention, the source components are used in the following weight ratio: resin:air:water:sulfuric acid = 1:(0,2-0,6):(0,7-1,0):(0,007-0,018). Optimal is the following mass ratio of initial components - resin:air:water:sulfuric acid = 1:0,35:1:0,007. The aqueous layer after phase separation of the mixture once used for blending with other source components. As water can be used pozharkovshchina water. The best result is achieved when the components are mixed at a temperature of 25°C, if this is m for mixing all of the components serves at the same time, and mixing are in the turbulent regime for a period of not more than 1 min with subsequent phase separation of no more than 30 minutes

The problem is solved also by the fact that in the plant for desalination of phenolic resin, comprising the device of mixing the starting components in connection with the device for phase separation of the mixture on the upper organic layer and a lower aqueous layer, the first output of which through the first accumulation tank and the pump is connected with a distillation device, which, through the fridge, the second container and the pump is connected with a mixing of the starting components, while the second output of the phase separation of the mixture through the third tank and the pump is also connected with a mixing of the starting components, and the second output of the distillation device is intended for removal of demineralized resin according to the invention, the device mixing the starting components is a mixer-turbulator made in the form of a metal pipe provided with at least three disks with holes, the disks are perpendicular to the pipe axis at a distance from each other with the formation of the mixing chambers (compartments), with the mixing chamber from the entrance is made with the ability to download all of the source components, and from the second output of the phase separation with whom thou hast made for allocation to reset the water layer. The unit can be equipped with a filter, the fourth pump and a fourth capacity, sequentially installed from the side of the second output device distillation. The holes in the disks have sizes and location, providing the possibility of creating a turbulent mode of mixing of the components in the mixing chambers of the. The area occupied by the holes is 40-60% of the surface area of the disk (without holes). In one embodiment of the mixer-turbulizer holes in the disks are located at the same distance from each other and from the Central axis. In the private embodiment, the first mixing chamber mixer, turbulizer has four inputs for the individual load components of the mixture - of phenolic resins, diisopropyl ether, water and concentrated sulphuric acid.

The claimed group of inventions is illustrated by drawings, where figure 1 shows the schematic diagram of the inventive installation, Fig 2 - disk for turbulent mixing of the components. Positions indicated on drawings: 1 - mixer-turbulization, 2 - device phase separation of the mixture on the upper organic layer and a lower aqueous layer, representing the Florentine vessel, 3, 6, 10 and 14 - capacity, 4, 7, 11 and 13 - pumps, 5 - node extraction production of phenol and acetone, 8 - distillation device made in view of the distillation column, 9 - refrigerator, 12 - filter.

Method of desalting phenolic resin includes a continuous multistage extraction process salt water and steam condensate, which is carried out on the installation (see figure 1, 2). In the mixer-turbulization 1 simultaneously serves phenolic resin, ether, water and concentrated sulfuric acid at a mass ratio of resin:air:water:sulfuric acid= 1:(0,2-0,6):(0,7-1,0):(0,007-0,018), in particular, when the mass ratio of resin:air:water:sulfuric acid = 1:0,35:1:0,007. Mixer-turbulization is a metal pipe which is provided with at least three disks with holes. The disks are perpendicular to the pipe axis at a distance from each other with the formation of four mixing chambers (compartments). When downloading the source components is performed via separate inputs for each component executed in the first mixing chamber. In the process of moving the mixture through the compartments is the mixing of the components, while turbulent mixing of the components of the moving stream is created in each subsequent compartment due to the separation of flow holes of the disk. A constructive solution used in the installation of the mixer-turbulizer provides a more effective molecular contact of the components with stirring in the turbulent regime.

Mixed in the mixture is body-turbulator 1 in the turbulent regime, the mixture is continuously fed in the Florentine vessel 2, the volume of which provides the total residence time of the mixture over 1 hour, where for less than 0.5 hours continuously is phase separation of the mixture on the upper organic layer and a lower aqueous layer. The Florentine vessel 2 by adjusting the shut-off valves (not shown) is continuously output from the upper organic layer of the holding tank 6, and the aqueous layer is the holding tank 3. With a capacity of 6 organic layer pump 7 served in the distillation column 8, where the upper part is disposed pairs of ether are cooled in the refrigerator 9 and enter the holding tank 10. The accumulation of air in the storage tank 10 by pump 11 is fed into the mixer-turbulization 1 for desalination of the phenolic resin. With distillation columns 8 desalted phenolic resin after filtration of solids on the filter 12 by a pump 13 serves the holding tank 14. The accumulation of water layer in the tank 3 pump 4 is fed into the mixer-turbulization 1 for desalination of the phenolic resin. The aqueous layer from the tank 3 is used in the desalting process only once and after demineralization of the Florentine vessel 2 aqueous layer is sent to the node extraction production of phenol and acetone 5.

The resulting demineralized resin has a high degree of purity with content (%, mass.): the sodium ion is not more than 0,0005) is - not more than 0.2, coke - not more than 2.2, ash - not more than 0.05, and does not contain other mineral salts, solids and water. Demineralized resin has an acid pH units 7-10 and viscosity almost 3.5 times lower than the original phenolic resin. Qualitative indicators desalted phenolic resin corresponds to the characteristics of the best boiler fuel - talk to the oil brand F according to GOST 10585-75 "Oil. Fuel oil". Chromato-mass-spectrometric method is investigated and it is shown that the combustion desalted phenolic resin in the composition of the flue gases, there is no such harmful substance, such as dioxin.

Comparison of the mass ratio of the resin components:air:water = 1:0,9:0,6 used in the known method (prototype), with the mass ratio of the components resin:air:water:sulfuric acid= 1:(0,2-0,6):(0,7-1,0):(0,007-0,018) or the optimal mass ratio of resin:air:water:sulfuric acid = 1:0,35:1:0,007 according to the claimed technical solution shows the cost savings of ether and water. The mass ratio of resin and ether 1: (0,2-0,6) is optimal to reduce the viscosity of the resin and the extraction of salt water from the resin with effective molecular contact of the components in the mixer-turbulator 1 in the turbulent regime. Further reduction of the ester is less than 0.2 mass units per unit weight of phenolic resin result is to increase the viscosity of the resin mixture:ether, that reduces the efficiency of extraction of salt water from a phenolic resin. In the known technical solution for 1-th level is the mass ratio of resin and water of 1:0.6 and additionally used the same amount of steam condensate at the last stage desalting resin or per unit mass of phenolic resin total flow of "fresh" water is 1.2 mass units of water or 1:1,2. In the claimed group of inventions in the total water consumption is 1 unit weight 1 unit mass of resin or 1:1 due to the use of single-stage desalting process even without considering her repeated single use, i.e. reduced water consumption due to efficient molecular contact of salt, resin and water in the turbulent regime of mixing in the mixer-turbulator 1 (see figure 1), which also allows the desalting process at a low temperature of 25°C.

The claimed group of inventions contains a set of essential features and advantages, such as more mass ratio of the components, a different sequence of operations and conditions of the implementation process, including the mode of mixing of the starting components, and other instrumentation used to obtain desalted phenolic resins of high purity.

In accordance with the declared technical features have been made, the setup is as for desalting phenolic resin capacity of 1-2 m 3/h Mixer-turbulization 1 made in the form of interconnected four pieces of a metal tube with an inner diameter of 100 mm, a thickness of 6 mm and a total length of 1000-1200 mm Pieces of pipes are connected by means of flanges with a diameter of 140 mm, between which there is a disk with a diameter of 112 mm, each of which is made with three holes with a diameter of 40 mm, spaced at the same distance from each other and from the Central axis of the disk (see figure 2) for passage of the mixture of initial components and creating a turbulent mode of mixing of the components. Cut pipes with disks form a mixing chamber (compartments). The first camera has four inputs to download the source components, the last camera is equipped with access for removal of the mixture components. Mixer-turbulization 1 is made of steel 12X18H10T. The disc material is Teflon or mixed steel 12X18H10T.

Florentine vessel 2 is a tank with a capacity of 12 m3with the cone-shaped portion of 3 m3and has a siphon for introduction of the mixture components from the mixer, turbulizer 1. Volume Florentine vessel 2 provides the total time of the mixed mixture components for more than one hour. The actual time of phase separation stirred mixture is less than 0.5 hour. Cumulative capacity of 3, 6, 10 and 14 represent qi is indijskie apparatus with a capacity of 6 m 3. Material Florentine vessel 2 and the vessel 3 is a steel 12X18H10T, and tanks 6, 10 and 14 steel 3. The pumps 4 and 11 represent the electric pump units of the type NDM dosing with adjustable flow and capacity 2000 l/h, the Material flow of the pumps HIT. Distillation column 8 is made of steel material 3 and represents the column with one nozzle plate, has a diameter of 800 mm and a height of 10000 mm Refrigerator 9 is a horizontal shell-and-tube apparatus with the surface of the heat transfer 26 m2with a diameter of 600 mm and a length of 2630 mm of material 12X18H10T. The pumps 7 and 13 are centrifugal pumps brand 1,25X-2K performance 3.2 m3/h and a pressure of 40 m water column. Material 12X18H10T.

Practice shows that in industrial conditions in the supply of components to the mixture instead of mass ratios of components it is convenient to operate volumetric ratio or volumetric flow rates of the components of the dosing pumps. When the density of the phenolic resin 1,08 g/cm3, ether 0,72 g/cm3water and 1.00 g/cm3and concentrated sulfuric acid to 1.83 g/cm3for well-known inventions mass mixing ratio resin:air:water = 1:0,9:0,6 corresponds to a volume mixing ratio of 1:1,3:0.6mm. In the proposed invention the mass aspect] is the solution of the resin components:air:water:sulfuric acid= 1:(0,2-0,6):(0,7-1,0):(0,007-0,018) corresponds to the volume ratio of resin:air:water:sulfuric acid= 1:(0,3-0,8):(0,7-1,0):(0,004-0,010), and the optimal mass ratio of the components resin:air:water:sulfuric acid = 1:0,35:1:0,007 corresponds to the optimal volume ratio of the resin components:air:water:sulfuric acid = 1:0,5:1:0,004. Therefore, in the following examples used the volumetric ratio of the components according to volumetric flow rates of components in m3/h dosing pump-mixer-turbulization 1.

In tables 1 and 4-6 presents examples of implementation of technical solutions, as in tables 2 and 3 characteristics desalted phenolic resin, clearly demonstrating the advantages of the proposed technology of desalting to obtain purified phenolic resins of high purity.

Examples 1-9.

Desalted phenolic resin with a content of sodium ions 0,013-0,014% wt. at the optimum mass ratio of the components resin:air:water:sulfuric acid = 1:0,35:1:0,007, which corresponds to the optimum volumetric ratio of resin components:air:water:sulfuric acid = 1:0,5:1:0,004 (table 1). For desalination of the phenolic resin used pourkashiyan water. Volumetric flow rate of phenolic resins, ether, water and concentrated sulfuric acid in a mixer-turbulization 1, respectively, 1 m3/h, 0.5 m3/h, 1 m3/h and 0,004 m3/H. the total volume flow of the mixture components in sosite the ü-turbulization 1, respectively 2,504 m 3/h mixing Time of these components in the turbulent regime in the mixer-turbulator 1 (see figure 1) was 45 sec. Total time of the mixed mixture components in the Florentine vessel 2 was 4 h, and the actual time of phase separation of mixed mixture components water and the organic layer Florentine vessel 2 was 10-16 min and did not depend on temperature in the range of 25-50°C (table 1). The output of the Florentine vessel 2 with a volume flow rate of the organic layer 1.5 m3/h and the aqueous layer 1.0 m3/h were carried out respectively in the storage tank 6 and 3. The aqueous layer contained 0,013-0,014% wt. sodium ions. Received desalted phenolic resin in quantities of 1 m3/h with the content of sodium ions is 0.0001-0,0005% wt. without mechanical impurities and water, with the characteristics listed in tables 2 and 3.

Desalted phenolic resin indicators comply with the requirements of THE 2424-020-05757601-98 "phenolic Resin" with the acidity of water extract in units of pH 6-10 and conditional viscosity almost 3.5 times lower than that of the original resin (table 2).

Received desalinated or purified from mineral salts, water and solids phenolic resin had a cocking behavior and sulfur content less than the best boiler fuel - bunker oil brand F according to GOST 10585-75 "Oil. Fuel oil is e" the ash content and the calorific value on the level with him and combustion in the flue gases was no harmful substances - dioxin (table 3). These parameters characterize the resulting desalted phenolic resin as a high-quality boiler fuel on the one hand, and on the other, as raw material for the production of technical carbon, and for the most rational way of its disposal - compositional modification of obtaining different products for technical purposes.

Examples 10-12

Desalting of the same phenolic resin was carried out at 25°C is similar to examples 1-9, only when the mass ratio of the components resin: air: water: sulfuric acid = 1:0,2:0,7:0,007, which corresponds to the volume mixing ratio resin:air:water:sulfuric acid = 1:0,3:0,7:0,004 (table 1), i.e. with lower levels of air and water per unit mass or volume of phenolic resin. This increased the actual time of the phase separation of aqueous and organic layer, which was 160-215 min or 2.7-3.6 hours (table 1). Reduction in the number of ether for 1 unit of mass or volume of phenolic resin has led to an increase in time of the phase separation of aqueous and organic layers by desalting phenolic resin. The final results are similar to examples 1-9.

Examples 13-17

Desalting of the same phenolic resin was carried out at 25-50°C (tab what Itza 1) analogously to examples 1-9, only when the mass ratio of the components resin:air:water: sulfuric acid = 1:0,6:0,7:0,007, which corresponds to the volume mixing ratio resin:air:water:sulfuric acid = 1:0,8:0,7:0,004, i.e. the amount of water was the same as in examples 10-12, while it increased the number of ether per unit mass or volume of phenolic resin. Compared to examples 10-12 actual time of the phase separation of aqueous and organic layer decreased, and it was the same as in examples 1-9 (table 1). Compared to examples 1-9 increase the number of ether per unit mass or volume of phenolic resin and temperatures up to 50°C did not significantly affect the time of phase separation. In connection with increase of the number of ether increased energy consumption during regeneration air at the distillation column 8 for reuse in the process. The final results are similar to examples 1-9.

Examples 18-22

Desalted phenolic resin with a content of sodium ions 0.026 and 0,033% wt. at 25°C (table 4) is similar to examples 1-9, only when content changes of concentrated sulfuric acid in a mass ratio of the components resin:air:water:sulfuric acid= 1:0,35:1:(0,0018-0,018) or in a volume ratio resin:air:water:sulfuric acid= 1:0,5:1:(0,001-0,010), where 1 m3/h phenolic resin, 0.5 m3/h ether and 1 m3/h water is served separately or, respectively, 0.001 m 3/h, or 0,002 m3/h, or 0,004 m3/h, or 0.005 m3/h or 0,010 m3/h of concentrated sulfuric acid (table 4). When applying sulfuric acid in a quantity of 0.001 m3/h and 0,002 m3/h was not clear phase separation. With weak or barely visible was the visible boundary of the phases the aqueous and organic layer and the aqueous layer was muddy, although the time of phase separation was small - 3-11 minutes When the supply of sulfuric acid in the amount of 0.004 m3/h, 0.005 m3/h and 0.010 m3/h showed a clear phase boundary water and the organic layer was decreased and the time of phase separation (table 4). When this aqueous layer was transparent. For desalting phenolic resin feed rate of sulfuric acid 0,004 m3/h was selected as optimum for optimum volumetric ratio of resin components:air: water:sulfuric acid = 1:0,5:1:0,004 or optimal mass ratio of the resin components:air: water:sulfuric acid = 1:0,35:1:0,007. The final results are similar to examples 1-9.

Example 23

Desalted phenolic resin with a content of sodium ions 0,034% wt. at 25°C (table 5) with the optimal mass ratio of the components resin:air:water:sulfuric acid = 1:0,35:1:0,007 or at the optimum volumetric ratio of resin components:air:water:sulfuric acid = 1:0,5:1:0,004 (table 1) anal is Gino examples 1-9, only instead pojarogasiteli water used repeatedly aqueous layer from the storage tank 3 containing original 0,034% wt. sodium ions. With increasing frequency of use or return water layer of the storage capacitor 3 in the desalting process each time a new batch of phenolic resin was increased phase separation from 12 min to 70 min, and increased content of sodium ions in the water layer from the initial values 0,034% wt. to 0,171% wt.(table 5). However, although slightly increased and the residual content of sodium ions from 0.0003 to 0,0008% wt. in desalted phenolic resin. The final results are similar to examples 1-9.

Example 24

Desalted phenolic resin with a content of sodium ions was 0.026% at 25°C (table 6) with the optimal mass ratio of the components resin:air:water:sulfuric acid = 1:0,35:1:0,007 or at the optimum volumetric ratio of resin components:air:water:sulfuric acid = 1:0,5:1:0,004 (table 1) is similar to examples 1-9 and example 23, when this monitored interface of the phases the aqueous and organic layers, appearance or condition of the water layer at re-used in the process of demineralization of phenolic resin. In all cases, the feed rate of sulfuric acid was 0,004 m3/h and was constant. When using aq the layer with the content of sodium ions 0,026% of the cumulative capacity 3 once in the process of demineralization of phenolic resin phase boundary water and the organic layer was clear, and the aqueous layer was transparent. When reusing water layer with the content of sodium ions 0,045% (table 6) for desalting phenolic resin interface of water and the organic layer was fuzzy, the aqueous layer was muddy. Therefore, in the future, the aqueous layer of the storage capacitor 3 is used only once, and after using it in the desalting process or the resulting aqueous layer with a content of sodium ions is more of 0.045% (table 6) with Florentine vessel 2 were dropped at the node extraction production of phenol and acetone 5. The final results are similar to examples 1-9.

Thus, examples 1-17 and 20-22 at mass mixing ratio resin:air:water:sulfuric acid= 1:(0,2-0,6):(0,7-1,0):(0,007-0,018), and in the best case scenario, when the mass ratio of resin:air:water:sulfuric acid = 1:0,35:1:0,007 show the effectiveness of the proposed technical solutions for desalination phenolic resin with obtaining purified phenolic resins of high purity content of sodium ions is not more 0,0006% of the mass.

Table 2
FeaturesThe original phenolic resinDesalted phenolic resin THE 2424-020-05757601-98
AppearanceViscous liquid dark colorViscous liquid dark colorViscous liquid dark color
Flashpoint10595Not below 62
The viscosity at 80°C, srvc. degrees4,61,3Not more than 5

Table 3
FeaturesThe original phenolic resinDesalted phenolic resinGOST 10585-75, requirements
Sulfur, %wt.0,3≤0,2≤0,5
Cocking behavior, %wt.5,0≤2,26,0
Ash content, %, mass.0,22≤0,05≤0,05
The warmth of the SG is Rania, kJ/kg3725440740÷4242040530
Dioxin in smoke. gases, ppmNo

Table 4
The time of separation, minThe organic layer, m3/hThe aqueous layer, m3/hThe appearance of the aqueous layer, the sharpness of the phase boundaryNa+in demineralized resin, %wt.Na+in the water layer, %, wt.Na+in the original resin, %wt.
H2SO4m3/h
180,00111Muddy, fuzzy
-----
190,0023Muddy, fuzzy
-----
200,00421,51,0Transparent, clear0,00010,0330,033
210,00511,51,0 Transparent, clear0,00010,0260,026
220,01040 sec1,51,0Transparent, clear0,00010,0260,026

Table 5
The multiplicity of the return water layer, the number of timesThe time of separation, minThe organic layer, m3/hThe aqueous layer, m3/hNa+in the water layer, %, wt.Na+in demineralized resin, %wt.
0121,51,00,0340,0003
1191,51,00,0680,0004
237 1,51,00,1030,0005
3401,51,0was 0.1380,0006
4701,51,00,1710,0008

Table 6
The multiplicity of the return water layer, the number of timesThe time of separation, minThe organic layer, m3/hThe aqueous layer, m3/hNa+in demineralized resin, %wt.Na+in the water layer, %, wt.The appearance of the aqueous layer, the sharpness of the phase boundaryH2SO4m3/h
021,51,0is 0.00020,026Transparent, clear0,004
121,51,0is 0.00020,045Transparent, clear0,004
221,5is 0.0002to 0.060Muddy, fuzzy0,004

1. A method of desalting a phenolic resin comprising mixing the starting components - phenolic resins, diisopropyl ether, water and concentrated sulfuric acid at a temperature of 20-60°C., phase separation of the mixture on top of the organic layer, which is a mixture of demineralized phenolic resin with ether, and the lower aqueous layer, followed by removal of the aqueous layer and distillation of the ether from the organic layer and obtaining desalinated phenolic resin, thus obtained ester is directed to the step of mixing the components, characterized in that the source components are used in the following weight ratio: resin:air:water:sulfuric acid= 1:(0,2-0,6):(0,7-1,0):(0,007-0,018), when this mixing is carried out in the turbulent regime.

2. The method according to claim 1, characterized in that the starting components used shall comply with the following mass ratio of resin:air:water:sulfuric acid= 1:0,35:1:0,007.

3. The method according to claim 1, characterized in that the aqueous layer after phase separation of the mixture once directed to the step of mixing the starting components.

4. The method according to claim 1, characterized in that the quality of water used pourkashiyan water.

5. The method according to claim 1, characterized in that the mixture of components is carried out at a temperature of 25°C.

6. The method according to claim 1, characterized in that mixing all of the components serves at the same time.

7. The method according to claim 1, characterized in that the components are mixed in the turbulent regime is carried out for not more than 1 min with subsequent phase separation of no more than 30 minutes

8. Installation for the desalination of phenolic resin according to claim 1, comprising a device for mixing the starting components in connection with the device for phase separation of the mixture on the upper organic layer and a lower aqueous layer, the first output of which through the first accumulation tank and the pump is connected with a distillation device, which, through the fridge, the second container and the pump is connected with a mixing of the starting components, while the second output of the phase separation of the mixture through the third tank and the pump is also connected with a mixing of the starting components, and the second output of the distillation device is intended for removal of demineralized resin, characterized in that the device offset ishonmaganhttp is a mixer-turbulization, made in the form of a metal pipe provided with at least three disks with holes, the disks are perpendicular to the pipe axis at a distance from each other with the formation of the mixing chambers, the first chamber from the entrance is made with the ability to download all of the original components from the second output of the phase separation of mixtures made for allocation to reset the water layer.

9. Installation according to claim 8, characterized in that it is equipped with a filter, the fourth pump and a fourth capacity, sequentially installed from the side of the second output device distillation.

10. Installation according to claim 8, characterized in that the holes in the disks have sizes and location, providing the possibility of creating a turbulent mode of mixing of the components in the mixing chambers.

11. Installation according to claim 8, characterized in that the holes in the disks are located at the same distance from each other and from the Central axis.

12. Installation according to claim 8, characterized in that the area occupied by the holes is 40-60% of the surface area of the disk.

13. Installation according to claim 8, characterized in that the first mixing chamber has four inputs for the individual load components of the mixture - of phenolic resins, diisopropyl ether, water and concentrated sulfuric acid.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: said compound is a clear phenol antioxidant from 2,6-di-tert-butyl-phenol through successive aminomethylation, hydrogenolysis and extraction of the desired product. The process is carried out in the presence of 2,6-di-tert-butyl-phenol and 2,4-di-tert-butyl-phenol in amount of 0.015-0.04 wt % and 0.1-0.2 wt % respectively, to the initial 2,6-di-tert-butyl-phenol.

EFFECT: method enables to obtain a compound having guaranteed colour index for a long storage period.

1 tbl, 7 ex

FIELD: chemistry.

SUBSTANCE: invention refers to method of reaction of alkene(s) contained in hydrocarbon stream, and in a reaction-rectifying system provided with rectifying sections and in between reaction zones with subnatant catalyst. The fluid is poured from the top of each overlying zone to the bottom of underlying zone. It is followed with partial disperse passing of vapour flow from underlying zone through each reaction zone. Thus residual vapour flow from each underlying zone is backflow to the top of overlying reaction zone through overflow space to poured fluid. As a rule, higher-boiling reagent is nontertiary alcohol, carboxylic acid or benzene, while essential reaction product is ether, ester or alkylbenzene.

EFFECT: improved method.

7 cl, 3 dwg, 6 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for preparing hydroxyaromatic compounds by oxidation of aromatic compounds with nitrous oxide in gaseous phase in the presence of zeolites. Method is realized by interaction of aromatic compounds of the formula (I): Ar-Rn wherein Ar means benzene or naphthalene; R means bromine, chlorine, fluorine atom, -NO2, -CN, -NH2, hydroxy-group, alkyl with 1-6 carbon atoms or phenyl; n = 0, 1 or 2 with nitrous oxide in gaseous phase in the presence of zeolites taken among the following order: pentasil, ferrierite and zeolite-β. Zeolite crystallites size is less 100 nm that is calcined before using at temperature from 500°C to 1350°C for 0.5-18 h. Before the calcination process zeolite is modified preferably by precipitation of silane or borane. Method provides realization of the process for a single step with high yield of the end compound and minimal formation of by-side substances.

EFFECT: improved preparing method.

11 cl, 3 tbl, 13 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to phenolic compounds, derivatives of dialkoxyethanals that are intermediate substances in organic synthesis and can be used as cross-linking agents of phenolic type no evolving formaldehyde also. Phenolic compounds are described of the general formula (I):

wherein: R means (C3-C17)-dialkoxymethyl, 1,3-dioxolan-2-yl substituted possibly at positions 4 and/or 5 with one or some (C1-C8)-alkyls, or 1,3-dioxane-2-yl substituted possibly at positions 4 and/or 5, and/or 6 with one or some (C1-C8)-alkyls; n = 1, 2 or 3, and group or groups of the formula: -CH(OH)-R are at ortho-position and/or at para-position with respect to OH in the cycle group; m = from 0 to 4-n; X means the functional group, such as OH or Hal, or (C1-C8)-alkyl, or (C1-C8)-alkoxyl, or (C5-C12)-aryl comprising in the known cases 1 or 2 heteroatoms, such as nitrogen or oxygen, or carboxy-group, or the group -CO-Y wherein Y means (C1-C8)-alkyl or (C1-C8)-alkoxyl, or amido-group, or amino-group, or thiol-group under condition that at least on of ortho- or para-positions in phenol cycle must be substituted with hydrogen atom, and their salts with alkaline metals, earth-alkaline metals and amines also. Method for preparing indicated phenolic compounds involves interaction of the corresponding substituted phenol wherein at least one ortho- or para-position in phenol cycle must be substituted with hydrogen atom with substituted aldehyde in the presence of a base. Invention provides preparing new compounds that can be used as cross-linking agents no evolving formaldehyde and as intermediate compounds used in organic synthesis.

EFFECT: improved method for preparing.

13 cl, 1 dwg, 10 ex

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention relates to a method for synthesis of phenols alkylated at ortho-position as parent substances used in preparing organic compounds. Method for preparing o-alkylphenols is carried out by interaction of phenol with alkanol at increased temperature in gaseous phase in the presence of metal oxide as a catalyst. Process is carried out for at least two stages in the molar ratio alkanol : phenol about ≤0.4, preferably, from 0.2 to 0.4 at each stage. Methanol is used as alkanol usually using aluminum gamma-oxide as a catalyst and process is carried out at temperature 300-400°C. Reaction products are separated by distillation. Invention provides increasing yield the end product due to enhancing selectivity with respect to o-alkylphenol.

EFFECT: improved method for preparing.

9 cl, 4 tbl, 2 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to preparing antioxidants of phenolic type. Method involves using alkylation products of mixture of para- and ortho-isomers of isononylphenol with isobutylene as an antioxidant. Alkylation reaction is carried out at 40-120°C and 0.02-0.4 MPa in the presence of acid catalyst in batch and continuous feeding isobutylene to reactor unit providing maintaining isobutylene concentration in reaction mass 0.8 mole/l, not above, and the total amount of isobutylene feeding to alkylation 1.82-2.0 mole per 1 mole parent alkylphenols. Method provides preparing antioxidant showing good technological properties and high effectiveness of protective effect for rubbers of emulsion polymerization and rubbers based on thereof, and simple method for its synthesis also.

EFFECT: improved method for preparing.

6 cl, 3 tbl, 7 ex

The invention relates to a method of selective oxidation of aromatic compounds (e.g. benzene and its derivatives) in gidroksilirovanii aromatic compounds (for example, into the corresponding phenols)

The invention relates to a method of allocation of ALKYLPHENOLS, in particular, para-tert-butylphenol (PTBP) from reaction mixtures

The invention relates to a method for the synthesis of alkyl phenols of General formula

< / BR>
where R is a tertiary CnH2n+1c n=4-8, 10 and Deut - C10H21

The invention relates to medicine, namely dentistry

FIELD: chemistry.

SUBSTANCE: process includes resorcinol extraction with organic solvent tributyl phosphate (TBPh). The well-milled hard foamed polyurethane (FPU) will be modified at that with tributyl phosphate in the mass ratio FPU:TBPh = 1:(2.0-2.5), the extraction will be performed prior to establishing the interphase balance with subsequent isolation of organic phase from the water phase.

EFFECT: process enables one to enhance the concentrating coefficient and reduce expenditure of the organic solvent tributyl phosphate.

1 tbl, 2 ex

The invention relates to pharmaceutical and food industry and for the allocation of biologically active substances from plant material

The invention relates to methods of cleaning product of phenol, the resulting acid-catalytic decomposition of cumene gidroperekisi

The invention relates to petrochemical technology, namely the production of phenol and acetone Kukolnik method

The invention relates to the processing and disposal of waste production of phenol and acetone, in particular to the desalting phenolic resin

FIELD: chemistry.

SUBSTANCE: process includes resorcinol extraction with organic solvent tributyl phosphate (TBPh). The well-milled hard foamed polyurethane (FPU) will be modified at that with tributyl phosphate in the mass ratio FPU:TBPh = 1:(2.0-2.5), the extraction will be performed prior to establishing the interphase balance with subsequent isolation of organic phase from the water phase.

EFFECT: process enables one to enhance the concentrating coefficient and reduce expenditure of the organic solvent tributyl phosphate.

1 tbl, 2 ex

FIELD: chemistry.

SUBSTANCE: present invention relates to a method for desalination of phenol resin and apparatus to that end. The disclosed method involves mixing starting components - phenol resin, diisopropyl ether, water and concentrated sulphuric acid at temperature 20-60°C, phase separation of the mixture into a top organic layer, which is a mixture of desalinated phenol resin and ether, and a bottom aqueous layer with subsequent removal of the aqueous layer and distillation of ether from the organic layer and obtaining desalinated phenol resin, wherein the obtained ether is fed to the step for mixing components. The starting components are used in the following weight ratio: resin : ether : water : sulphuric acid = 1 : (0.2-0.6) : (0.7-1.0) : (0.007-0.018), wherein mixing is carried out in turbulent conditions.

EFFECT: present invention enables to obtain desalinated resin with high degree of purity while reducing the cost of the process and the obtained product.

13 cl, 24 ex, 6 tbl, 2 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a novel method of producing fullerenol C84, wherein dry carbon sludge (carbon nano-cluster sulpho-adduct production wastes) is fed into Soxhlets extraction apparatus and fullerenol is extracted in form an aqueous solution of an ammonia salt of fullerenol using an ammonia solution and heating in the evaporation part of the extraction apparatus.

EFFECT: method enables to recycle sulpho-adduct production wastes to obtain fullerenol C84.

12 cl, 3 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of concentrating pyrocatechol from aqueous solutions, which includes concentrating pyrocatechol from aqueous solutions acidified to pH=1-5 at temperature of 20±2°C with an organic solvent. The organic solvent used is tributyl phosphate in hexane, which is deposited on elastic polyurethane foam with weight ratio of the elastic polyurethane foam to tributyl phosphate of 1:(0.5-0.75).

EFFECT: method increases the concentration factor and degree of extraction of pyrocatechol and reduces consumption of the organic solvent.

1 tbl, 3 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to preparing antioxidants of phenolic type. Method involves using alkylation products of mixture of para- and ortho-isomers of isononylphenol with isobutylene as an antioxidant. Alkylation reaction is carried out at 40-120°C and 0.02-0.4 MPa in the presence of acid catalyst in batch and continuous feeding isobutylene to reactor unit providing maintaining isobutylene concentration in reaction mass 0.8 mole/l, not above, and the total amount of isobutylene feeding to alkylation 1.82-2.0 mole per 1 mole parent alkylphenols. Method provides preparing antioxidant showing good technological properties and high effectiveness of protective effect for rubbers of emulsion polymerization and rubbers based on thereof, and simple method for its synthesis also.

EFFECT: improved method for preparing.

6 cl, 3 tbl, 7 ex

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