Method of desalting phenolic resin

 

(57) Abstract:

Usage: cleanup from salts of phenolic resins - waste production of phenol and acetone through Gidropress cumene. The inventive phenolic resin diluted with water and diisopropyl ether or cumene wt. the ratio of resin: ether: water = 1 : 0,9 : 0.6mm or resin: isopropyl: water is 1 : 1.5 : 0.6 and lead extraction with water at 20 - 60oWith in a few steps, and one of the intermediate steps add sulfuric acid to pH of the organic layer is not more than 7. Provide recycling water layers. 1 C. p. F.-ly, 1 Il.

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

In the production of phenol and acetone Kukolnik method as waste is formed of phenolic resin or any of its fractions, which contain up to 2 wt. mineral salts and solids.

It is known that most of the methods of processing and utilization of phenolic resins require prior purification of salts. Desalted product of a different degree of purification can be used in the production of carbon black, coke, phenol-formaldehyde resins, bit the thief sulfuric acid [1 and 2]. In this part present in the phenol resin salts, representing the reaction of sodium and iron, is transformed into a salt of sulphuric acid, together with the main mass of sodium sulfate is transferred to the aqueous solution of sulfuric acid. The process is carried out at 50-60aboutC. the ratio of the phenolic resin and the acid solution is 1-0,5 volume.

The disadvantages of the proposed method of desalting phenolic resins include the following:

the use of large quantities of sulfuric acid, the appreciation of the process;

the emergence of a large number of industrial wastewater contaminated by the products of the neutralization of sulfuric acid;

increased corrosion of the process equipment, the need for expensive corrosion resistant coating.

In order to ensure more environmentally friendly technologies that reduce the consumption of reagents such as sulfuric acid, neutralizing agent (NaOH, Na2CO3and others), reducing the risk of corrosion of the equipment, using simple and cheap materials for its manufacture a new method of desalination of phenolic resins by multistage extractive treatment of the resin with water in the presence of a solvent diisopropyl ether or isopropylbenzene (cumene).Ziya water in the presence of a solvent diisopropyl ether or isopropylbenzene at the following mass ratio of phenolic resin DIPA water 1:0,9:0,6, or phenolic resin: IPA water is 1:1.5:0.6mm. As water use steam condensate.

The ratio of costs phenolic resin, solvent and water depends on the composition of phenolic resin, the content of salts, choice of solvent and is determined by the need to maintain the calculated density and viscosity of the hydrocarbon and water phases in the separation tanks.

To avoid the formation of stable emulsions pH of the working environment in the desalting process should be no more than 7. Since the pH of the phenolic resin ranges from 5-10% provides periodic dosage of sulfuric acid in the zone of mixing the mixture of phenolic resin, solvent, and water.

The drawing shows the setup diagram for the implementation of the proposed method.

Phenolic resin in a quantity of 2500 kg/h and a temperature of 80-90aboutC goes to the refrigerator 1, which is water-cooled to 40-50aboutWith, and then is directed to a container with an agitator 2. In the pipeline phenolic resin or directly into a container with a stirrer 2 served continuously pump N 20 2250 kg/h diisopropyl ether from the intermediate tank 19. The level in the tank is kept constant and in the case of loss of DIPA in this capacity is Roy intensively mixed with water 2-stage extraction, which number 1150 kg/h is pumped by pump 6 from the tank 8. The resulting mixture flows into the Florentine vessel 7, which splits into two phases, organic, partially purified from salts, and water contaminated with salts and organic impurities. The aqueous phase is sent to the node wastewater from organic impurities.

Organic phase in the amount of 4750 kg/h comes in a container with a stirrer 5 where it is mixed with water the third stage of extraction. Water is fed by the pump 13 in the amount of 1500 kg/h from the tank 12. In a container with a stirrer is provided with an automatic feed of 93% sulfuric acid. The operation of automatic devices for sulfuric acid is associated with indications of a pH meter, which is determined by the pH of the medium in the vessel 8. From the tank with agitator 5 after intensive mixing, the mixture of phenolic resin, DIPE and water flows in the Florentine vessel 7. After stratification in the vessel, the aqueous phase by means of a device enters the tank 8, where the pump 6 is pumped to the first stage of extraction in a container with a stirrer 3. This creates a counter-current and saved the ratio between organic and aqueous phases. Organic phase in the amount of 4750 kg/h comes in clearly the ez refrigerator 10. With the help of the refrigerator 10 is provided for cooling the steam condensate from 90-95aboutWith up to 40-50aboutC. From the tank with agitator 9 mixture components flows into the Florentine vessel 11. After separation the aqueous phase in the amount of 1500 kg/h by means of a device flows into the tank 12, where the pump 13 is fed into the tank with agitator 5 to the second stage of extraction. The organic phase free of salt enters the tank 14, where the pump 15 is supplied to the power of the distillation column 16. The distillation of the solvent to produce the heating steam pressure of 15-16 kg/cm2through a remote boiler 17. To reduce losses DIPA with kubovy product (phenolic resin) in the lower part of the column serves 40-50 kg/h steam. Pair the top of the column is sent to a water heat exchanger where it is condensed and then collected in tanks 19. Some of them served as phlegmy in the upper part of the column, and the carrying amount of 2250 kg/h pump 20 pump in the initial part of the process flow for mixing with the original phenolic resin. This ensures recycling of the necessary quantity of solvent in order to provide a constant ratio between the phenolic resin and DIPA level 1-0,9 mass.

In the line% and its distillate to produce an additional vacuum distillation column.

Cubic liquid column 16 desalted phenolic resin is pumped by pump 21 to further processing or in the form of a commercial product sent to the warehouse.

The salt content of the phenolic resin at the exit of the facility is less than 0.01 wt. (the degree of purification 99,0% content of Na ions is not more of 0.003 wt. ).

For optimal temperature extraction were carried out laboratory tests. The test results are illustrated by examples.

P R I m e R 1. Phenolic resin density of 1.09 g/cm3and salt content 1,96 wt. in the amount of 100 g of pre-mix with 90 g DIPE and then treated with 60 g of water scheme is a three-stage countercurrent extraction at 20aboutC. the Ratio of components in each stage is kept in wt. shares within 1:0,9:0.6mm. The residual salt content in the organic layer 0.017 wt. in terms of phenolic resin. The degree of purification of salts of 99.1%

P R I m m e R 2. The process is carried out analogously to example 1, but the temperature of the extraction of the 60aboutC. purification of salts 98,7%

P R I m e R 3. The process is carried out analogously to example 1, but the temperature of the extraction of the 75aboutC. purification of salts of 97.4%

Lowering the temperature of extraction below 20

1. METHOD of DESALTING PHENOLIC RESIN continuous multistage extraction with water in the presence of sulfuric acid at 20 - 60oWith subsequent separation of the aqueous and organic layers, characterized in that the phenolic resin as the organic solvent previously added diisopropyl ether or isopropylbenzene, and sulfuric acid is metered at one of the intermediate stages of extraction in an amount to provide a pH of the organic layer is not more than 7, this system derive the main part of the aqueous layer after the first stage of extraction and provide recycling water layers in subsequent stages of extraction, in addition, the organic layer from the subsequent-stage extraction is sent to a distillation column, in which the solvent is separated from the demineralized resin and then reuse the first stage of extraction.

2. The method according to p. 1, characterized in that the extraction is carried out at a mass ratio of resin: diisopropyl ether : water = 1 : 0,9 : 0.6 or resin : cumene : water = 1 : 1,5 : 0.6mm.

 

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