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Study On Purification Of 1-Sulfonic Acid Cyclohexane Carboxylic Acid And Its Syntnesis Cyclohexane Carboxylic Acid

Posted on:2013-10-19Degree:MasterType:Thesis
Country:ChinaCandidate:Y P HeFull Text:PDF
GTID:2271330485995060Subject:Chemical Engineering and Technology
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The technology of the production of caprolactam from toluene in Sinopec Shijiazhuang refining enterprise introduces Italian SNIA company.Its production capacity of 170000 tons caprolactam and. the wastewater discharge of 100000 tons euery year. The technology production process complex, products more, produce waste complicated composition, mainly contain caprolactam, sulfur ammonium, acetic acid, toluene, benzoic acid, cyclohexane acid,1-sulfonic acid base cyclohexane carboxylic acid organic materials, belongs to the difficult to deal with high concentration organic wastewater, not directly emissions. At present the company of high temperature burning method to deal with the waste liquid, there are high in energy consumption, the high cost of operation, easy nozzle, waste valuable ingredients not recycling shortcomings. This experiment used boiling distillation method of the waste water, as separated into a coarse and have the motor oil, water treatment with flocculant to request directly emissions, by analyzing the coarse main composition is 1-sulfonic acid base cyclohexane carboxylic acid, and carries on the synthesis refining and purification ring has the formic acid.Experimental studies showed that:the boiling distillation separation method of caprolactam waste liquid in toluene as were boiling agent, will waste liquid water, coarse for separation and oil. Sure were boiling agent and waste liquid mass ratio of 1:2, the temperature of 103℃ were boiling,, water yield 52.25%, with the boiling distillation get by methanol phosphate-contained residue after washing, get coarse and methanol fluid, liquid methanol by distilling, recycling get methanol recycling, boiling agent of toluene recycling use, the burning hot oil determination for 20 384J/g, w(s)=1.07%, sulfur is not high, achieve furnace with fuel oil (heavy oil) technology index, the desulphurization processing, can be used for boiler, kiln for fuel use etc. The boiling water of distillation get, after testing COD as high as 7270 mg/L, not directly emissions, experiment used inorganic flocculant polyferric sulphate and organic flocculants polyacrylamide with way processing, on polyferric sulphate dosing quantity 0.1 g/L, PAM dosing quantity 0.05 g/L COD removal rate when reached 90%, basic to reach company emissions requirements. Coarse by HPLC analysis the main composition is 1-sulfonic acid base cyclohexane carboxylic acid, the active carbon adsorption-acid crystallization chromatography purification of refined, get 1-sulfonic acid base cyclohexane carboxylic acid purity of 99.8%, the yield is 84.8%. Discusses the active carbon adsorption technology kind and amount of activated carbon, the solution pH value, adsorption time and acid analysis process of sulfuric acid adding quantity conditions on the 1-sulfonic acid base cyclohexane carboxylic acid purity and yield of influence, and in the 95 g coarse solution, activated carbon dosage 1.0 g, solution initial pH=6, adsorption time 60 min, strong sulfuric acid dosing quantity 8 g, purification and get the 1-sulfonic acid base cyclohexane carboxylic acid high purity, and use infrared and nuclear magnetic resonance (NMR) confirmed the structure. Use of the history of NiFanYing products to 1-sulfonic acid base cyclohexane carboxylic acid of processing, in the material ratio, temperature and reaction time investigation can be concluded that:in the 150 ℃, with rare sulfuric acid hydrolysis for medium,,1-while the cyclohexane in autoclave carboxylic acid inside can take off sulfonic acid base, generating cyclohexane carboxylic acid.
Keywords/Search Tags:caprolactam waste liquid, 1-sulfonic acid base cyclohexane carboxylic acid, purification process, activated carbon
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