Method of desalting phenolic resin

 

(57) Abstract:

Usage: remove salts of phenolic resins-waste production process the production of phenol and acetone through Gidropress of cumene. The inventive desalting phenolic resin lead extraction in an aqueous solution of diisopropyl ether at 60oAnd the mass ratio of resin: ether 1:(0,5-1,5):(0,3-0,9), then salt water layer separated from the organic layer . table 2.

The invention relates to a method of desalting a phenolic resin obtained in the process of co-production of acetone and phenol Kukolnik method, and can be used in the processing of phenolic resins.

Phenolic resin contains the following components: phenol, acetophenone, dimethylphenylcarbinol, cumylphenol, the dimer-methylstyrene and heavier condensation products. The percentage of these components depends on the quality of raw materials used and the process conditions. The salt content in the resin is from 0.5 to 2.5 wt. For most of the methods of processing of phenolic resins such salt content is unacceptable.

Known industrial method [1] desalting the dryer is the same.

The process is carried out as follows:

Phenolic resin allocated for desalination, handled 10% solution of sulfuric acid (for dilution of concentrated sulfuric acid is used steam condensate) in a volume ratio of the resin-solution of sulfuric acid is 1:0.5 in. The processing time is 60 minutes After the treatment solution is asserted for 2 h and demineralized resin with the remnants of the sulfuric acid is supplied to the washing from acid water. Uses two stages of contact. At each step the ratio of water-resin is 0.5:1. The length of time of the processing water is 30 min, and the length of time the separation of a mixture of water-resin 3 hours the Process is carried out at 60aboutC. the Degree of extraction of salts was 85-90%

The disadvantages of the method include the low degree of extraction of salts; the use of relatively expensive alkali to neutralize the acid; the significant costs of water for the two-stage washing from sulfuric acid; the use of steam condensate to dilute sulfuric acid, which reduces the degree of heat recovery, the long duration of treatment and separation of mixtures, resulting in low volumetric speed of the process.

The aim of the invention autokey extraction with water in the presence of diisopropyl ether.

The process of demineralization of phenolic resin is as follows.

Phenolic resin allocated for desalination, mixed with diisopropyl ether (DIPE) in the ratio of 1:(0.5 to 1.5) and with a part of water (15-20% of the total amount of water) from the bottom of the separation zone of the extraction column and enters the emulsifier, where intensively stirred for 3-5 min, and then separated in the demulsifier. The time separation 5-10 minutes the Top layer of the demulsifying agent containing a resin with DIPE, is sent to the extraction column to achieve the required degree of desalting resin, and the bottom layer containing water with salts, combined with the extract phase at the bottom of the separation zone of the column. In the extraction column of water so that the ratio of resin-DIPA water was equal to 1:(0,5-1,5):(0,3-0,9). Raffinata phase containing demineralized resin with DIPE, is fed to the rectification for distillation of DIPE and extract phase containing water, salts and dissolved organic nitrogen (mainly phenol) on site sewage treatment.

P R I m e R 1. Phenolic resin containing 0.5 wt. salt, is subjected to a single extraction, for which purpose it is mixed with DIPE in flask thermostated at 60aboutWith and in contact with bootsthat to full lamination (5 min) and divided into two phases afromontane and water-salt. The original resin, the raffinate and the extract was analyzed for salt content by the method of combustion with a gradual increase in temperature up to 600aboutC.

The degree of extraction of salts was calculated as

100 where xwith(Ref.)the salt concentration in the original pitch;

xc(c.c.)the salt concentration in demineralized resin.

The distribution coefficient of the salt was calculated as

Kcwhere xc(C. c.)the concentration of salt in the water-salt layer

In this example,

100=85%

Kc9,44

P R I m e R s 2-6. Experiments are performed in the same way as in example 1, but for extraction were used samples of resin with a salt content of 0.32; 0,54; 1,38; 1,95 and 2.57 wt. The results obtained are presented in table.1. Component resin compositions obtained by gas chromatography analysis are given in table.2.

P R I m e R s 7-11. Experiments for samples of resin containing 0,32; 0,50; 1,38; 1,95 and 2.57 wt. salts, carried out as described in example 1, but the mixing is carried out for 60 minutes, the Obtained results are presented in table.1.

P R I m e R s 12-15. For samples of resin containing 0,38; 1,38; 1,95 and 2.57 wt. salts, the extraction was carried out as in example 1, but the mass ratio of the resin-DIPA-fly, containing 0,38; 1,95 and 2.57 wt. salts, the extraction was carried out as in example 1, but the mass ratio of the resin-DIPA-water ratio = 1:0,9:0,3. The results obtained are presented in table.1.

P R I m e R s 20-24. Samples of phenolic resin containing 0,38; 0,54; 1,38; 1,95 and 2.57 wt. salt is subjected to two-, three-extraction by re-extraction at 60aboutWith Pirosmani mixture with water after contact, sludge and separating the previous portions of water. Conditions for the allocation process and the results obtained are presented in table.1.

P R I m e R 25. Phenolic resin containing 2.57 m wt. subjected to three-stage countercurrent extraction at 60aboutWhen the ratio of resin-DIPA water equal to 1:1,5:0.6mm. The resulting resin with a salt content of 0.02 wt.

P R I m e R 26. Phenolic resin containing 1,95 wt. subjected to three-stage countercurrent extraction at 60aboutWhen the ratio of resin-DIPA water equal to 1: 0,9: 0.6mm. The resulting resin with a salt content 0,0008 wt.

P R I m e R 27. Phenolic resin containing 0.50 wt. salt is subjected to three-stage countercurrent extraction at 60aboutWhen the ratio of resin-DIPA water equal to 1: 0,9:0.6mm. The resulting resin with a content ode 10% solution of sulfuric acid and subsequent washing with water in two stages. Processing time and separation is the same as in the industrial prototype. The resulting resin with a salt content of 0.11 wt. The degree of extraction of salts was equal to 78%

P R I m e R 29 (comparative prototype). Sample resin containing 1,95 wt. salt, is subjected to desalting the same way as in example 28. The resulting resin with a salt content to 0.70 wt. The degree of extraction of salts was equal to 64%

P R I m e R 30 (for comparison, the lower limit on the water). Sample resin containing 0,38 wt. salt, is subjected to extraction as in example 1, but the mass ratio of the resin-DIPA-water ratio = 1:0,9:0,1, = 80,3% OFFwith4,08. The time separation of the phases, it is difficult to establish because the water layer had a color identical to the color of the organic layer.

P R I m e R 31 (for comparison, the lower limit on DIPA). Sample resin containing 0,38 wt. salt, is subjected to extraction as in example 1, but the mass ratio of the resin-DIPA-water ratio = 1:0,4:0,6, = 65,1% OFFwith6,02. The time separation of the phases is equal to 10-15 minutes

P R I m e R 32 (for comparison, the limit on temperature). Sample resin containing 0,38 wt. salt, is subjected to extraction as in example 1, but the temperature of extraction was equal to 40aboutWith, the tion aqueous solution at 60oWith subsequent separation of the mixture into aqueous and organic layers, characterized in that the extraction was carried out in the presence of diisopropyl ether at a mass ratio of resin ether water respectively 1,5 1 0,5 0,3 0,9.

 

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