FIELD: industrial organic synthesis.
SUBSTANCE: invention relates to production of isoprene for use in synthesis of isoprene rubber, butyl rubber, and isoprene-containing polymers used in tire industry and manufacture of general mechanical rubber goods. In the method of invention, isoprene is obtained by decomposition of 4,4-dimethyl-1,3-dioxan on calcium phosphate catalyst comprising synthesis of 4,4-dimethyl-1,3-dioxan by interaction of isobutylene-containing C4 fraction with formaldehyde-containing blend based on methanol-free formalin obtained by oxidation of methanol followed by rectification of formalin, accomplished at elevated temperature and pressure in presence of acid catalyst followed by separation of reaction medium into oil and water layers including extraction of organic products from water layer, isolation of 4,4-dimethyl-1,3-dioxan, unreacted C4-hydrocarbons, and high-boiling by-products from oil layer, condensation of 4,4-dimethyl-1,3-dioxan decomposition contact gas and isolating from condensate isoprene, unreacted 4,4-dimethyl-1,3-dioxan, recycling isobutylene and formaldehyde-containing water, performing also withdrawal of extracted water layer to be vacuum evaporated followed by sending evaporated water layer to preparation of formaldehyde-containing blend. Evaporation of extracted water layer containing acid catalyst is carried out at temperature of boiler wall in rectification column 80-105°C and residual pressure 0.015-0.025 MPa. Distillate is mixed with above-indicated formaldehyde-containing water and resulting mixture is subjected to two-step concentration of formaldehyde. Second-step distillate, namely recycle methanol, is sent to oxidation zone. Bottom residues of the second step of formaldehyde concentration and those of the extracted water layer evaporation are combined with methanol-free formaldehyde and acid catalyst continuously supplied as replenishment, after which used as formaldehyde-containing blend in the 4,4-dimethyl-1,3-dioxan synthesis. Concentration of acid catalyst is maintained between 1.60 and 1.75 wt %.
EFFECT: increased productivity and reduced material and power consumption.
2 cl, 1 dwg, 5 ex
Title | Year | Author | Number |
---|---|---|---|
METHOD FOR PREPARING ISOPRENE | 2003 |
|
RU2258690C1 |
ISOPRENE PRODUCTION PROCESS | 2003 |
|
RU2248961C1 |
ISOPRENE PRODUCTION PROCESS | 2003 |
|
RU2248959C2 |
ISOPRENE PRODUCTION PROCESS | 2004 |
|
RU2255928C1 |
METHOD OF ISOPRENE OBTAINING | 2014 |
|
RU2553823C1 |
METHOD OF PRODUCING ISOPRENE | 2011 |
|
RU2458900C1 |
ISOPRENE PRODUCTION PROCESS | 2004 |
|
RU2255929C1 |
METHOD FOR PREPARING 4,4-DIMETHYL-1,3-DIOXANE | 2004 |
|
RU2255936C1 |
METHOD OF PRODUCING 4,4-DIMETHYL-1,3-DIOXANE | 2010 |
|
RU2458922C2 |
METHOD OF PRODUCING ISOPRENE | 2014 |
|
RU2575926C1 |
Authors
Dates
2005-03-27—Published
2003-05-15—Filed