CN103539711B - A kind of technique being continuously separated pure compound from refinery's mercaptan removal waste liquid - Google Patents
A kind of technique being continuously separated pure compound from refinery's mercaptan removal waste liquid Download PDFInfo
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Abstract
The present invention discloses a kind of technique being continuously separated pure compound from refinery's mercaptan removal waste liquid, mercaptan removal waste liquid is sent to the first rectifier unit rectifying, after Methyl disulfide is separated, liquid at the bottom of the tower of the first rectifier unit is continued to send the second rectifier unit rectifying to, after methylethyl two sulphur is separated, send liquid at the bottom of the tower of the second rectifier unit to the 3rd rectifier unit rectifying, be separated diethyl two sulphur.Present invention achieves and isolate pure compound component from mercaptan removal waste liquid, the Methyl disulfide separated, methylethyl two sulphur, diethyl two sulphur product purity reaches more than 99% respectively, reach the specification of quality of pure compound, the product yield of production reaches more than 95%.
Description
Technical field
The present invention relates to the technique of separating compound, particularly relate to a kind of technique being continuously separated pure compound from refinery's mercaptan removal waste liquid.
Background technology
The liquefied petroleum gas (LPG) that refinery is produced all needs through mercaptan removal process before dispatching from the factory, and treatment process is for contacting with liquefied gas with alkali lye.Mercaptan in liquefied gas and the NaOH in alkali lye react and generate sodium mercaptides, the sodium mercaptides generated is dissolved in alkali lye, realize removing of mercaptan in liquefied gas, in doctor process in early days, when the NaOH in alkali lye consumes completely, alkali lye is conveyed to wastewater treatment equipment process, causes cost for wastewater treatment very large.In recent years, in Ningbo, a company develops alkali lye oxygen-rich oxide regeneration techniques, and many refinery application at home, the oxygen rich air that this technology utilizes refinery air separation facility to produce carries out oxidation regeneration to reacted alkali lye, and its chemical reaction process is:
2RSNa +
O
2+H
2O → R-S-S-R + 2NaOH
Regenerative process is that sodium mercaptides and oxygen reaction generate disulphide and NaOH, and disulphide and the alkali lye of generation are immiscible, after stratification, separation alkali lye, realizes alkali liquid regeneration and recycle.The waste liquid separated is mercaptan removal waste liquid, and its main component is disulphide.Due to the violent in toxicity that disulphide is a kind of high sulfur-bearing, as being dispersed in environment, can severe contamination be caused, therefore needing to do special processing, destroy its molecular structure to eliminate or to reduce toxicity.At present, refinery mainly processes by the method for burning, and this treatment process not only needs to drop into a large amount of processing costs, and burning process produces a large amount of sulfurous gas, still produces serious pollution to environment, fails the pollution thoroughly solved environment.
The technique preparing vulcanizing agent with the mercaptan removal waste liquid of alkali liquid regeneration by-product is disclosed in CN201210401963.3, this technique is simpler, productive expense is low, it is a kind of mercaptan removal waste water utilization method preferably, but the product application face of gained is narrower, absorption of market is limited, can not complete digestion refinery production process to produce be mercaptan removal waste liquid, a large amount of mercaptan removal waste liquids still awaits developing.
Summary of the invention
The object of this invention is to provide the technique being continuously separated pure compound from refinery's mercaptan removal waste liquid, this technique can be continuously separated the Methyl disulfide in mercaptan removal waste liquid, methylethyl two sulphur and diethyl two sulphur, the purity of each compound, more than 99%, can be used as pure compound product application.
The object of the invention is to be achieved through the following technical solutions: a kind of technique being continuously separated pure compound from refinery's mercaptan removal waste liquid, mercaptan removal waste liquid is sent to the first rectifier unit rectifying, after Methyl disulfide is separated, liquid at the bottom of the tower of the first rectifier unit is continued to send the second rectifier unit rectifying to, after methylethyl two sulphur is separated, send liquid at the bottom of the tower of the second rectifier unit to the 3rd rectifier unit rectifying, be separated diethyl two sulphur.
Containing following compound in mercaptan removal waste liquid: Methyl disulfide, methylethyl two sulphur, dimethyltrisulfide, diethyl two sulphur and other sulfide on a small quantity, simultaneously with the high-boiling-point impurity such as sodium hydroxide, semi-annular jade pendant phthalein cyanogen cobalt of trace, be summed up as metallic compound and the large class of nonmetallic compound two, the boiling spread of nonmetallic compound is between 108 DEG C ~ 165 DEG C, and the boiling point of metallic compound is more than 300 DEG C.The boiling point of Methyl disulfide is 109 DEG C, and the boiling point of methylethyl two sulphur is 131 DEG C, and the boiling point of diethyl two sulphur is 154 DEG C, and the boiling point of dimethyltrisulfide, for being greater than 170 DEG C, can adopt the method for fractionation to be separated the pure compound in mercaptan removal waste liquid.In the present invention, three rectifier units are adopted to be separated with dimethyltrisulfide Methyl disulfide, methylethyl two sulphur, diethyl two sulphur, in the distillation operation that each is concrete, according to respective operating features, tower top temperature, bottom temperature, tower certain some temperature interior can be selected as main control parameters.In the present invention first rectifying tower, owing to requiring that overhead product Methyl disulfide purity is more than 99%, require that the Methyl disulfide content of tower kettle product is below 0.5% simultaneously, but in operation, when the purity of overhead product occurs slightly to change, the reaction of tower top temperature is not obvious, operation can not be carried out according to tower top temperature to control, and when changing appears in the ratio of methylethyl two sulphur and diethyl two sulphur, in normal running, bottom temperature there will be change, therefore can not carry out operation according to bottom temperature and control.And when subtle change appears in overhead product purity, opening for feed vapor phase temperature has comparatively considerable change, and the impact of change on opening for feed vapor phase temperature of methylethyl two sulphur of raw material and diethyl two sulphur ratio is little, control opening for feed vapor phase temperature higher than tower top temperature certain limit, the separate targets of the first rectifying tower can be reached, thus select opening for feed vapor phase temperature as the main operation controling parameters of the first rectifying tower.Second distillation column operating features is similar to the first rectifying tower, also selects opening for feed vapor phase temperature as main control parameters.3rd rectifying tower selects bottom temperature as main control parameters, the object of the 3rd rectifying tower obtains the satisfactory overhead product of purity, tower kettle product is as waste disposal, control bottom temperature higher than tower top temperature certain limit, the purity of overhead product can be ensured, also ensure that tower reactor waste material can not lose too much diethyl two sulphur.In addition, Methyl disulfide, methylethyl two sulphur, diethyl two sulphur and dimethyltrisulfide are labile compounds, in operation, are also noted that the bottom temperature of each rectifier unit should be not too high, otherwise these compounds can decompose, affect the rate of recovery of each compound.
In view of the foregoing, the rectifying condition optimization of the first rectifier unit of the present invention is: rectifying tower rectifying section theoretical plate number: 23-28 block, rectifying tower stripping section theoretical plate number: the operation of 25-30 block, rectifying tower absolute pressure: 0.08-0.12Mpa, rectifying tower operating reflux ratio: 12-17 ﹕ 1, rectifying tower head temperature: 100-115 DEG C, rectifying tower opening for feed gas phase temperature: 105-130 DEG C, tower bottom of rectifying tower temperature: 125-145 DEG C.
The rectifying condition optimization of the second rectifier unit of the present invention is: rectifying tower rectifying section theoretical plate number: 23-28 block, rectifying tower stripping section theoretical plate number: 25-30 block, rectifying tower operation absolute pressure 0.02-0.04 Mpa, rectifying tower operating reflux ratio: 10-15 ﹕ 1, rectifying tower head temperature: 100-120 DEG C, rectifying tower opening for feed gas phase temperature: 105-135 DEG C, tower bottom of rectifying tower temperature: 120-145 DEG C.
The rectifying condition optimization of the 3rd rectifier unit of the present invention is: rectifying tower rectifying section theoretical plate number: 15-20 block, rectifying tower stripping section theoretical plate number: the operation of 15-20 block, rectifying tower absolute pressure: 0.01-0.03Mpa, rectifying tower operating reflux ratio: 6-10 ﹕ 1, rectifying tower head temperature: 110-130 DEG C, rectifying tower opening for feed gas phase temperature: 112-135 DEG C, tower bottom of rectifying tower temperature: 120-145 DEG C.
the present invention compared with prior art has the following advantages:
Present invention achieves and isolate pure compound component from mercaptan removal waste liquid, the Methyl disulfide separated, methylethyl two sulphur, diethyl two sulphur product purity reaches more than 99%, reach the specification of quality of pure compound, the product yield of production reaches more than 95%, and the three kinds of products produced due to the present invention are the huge product of market capacity, greatly widen the application of mercaptan removal waste liquid, the outlet of mercaptan removal waste liquid is solved preferably.Present invention employs rational temperature, pressure parameter, there is not material in process of production and decompose.
Accompanying drawing explanation
Fig. 1 is the structural representation of the continuous rectification system of employing of the present invention.
Embodiment
The continuous rectification system being continuously separated pure compound from refinery's mercaptan removal waste liquid as shown in Figure 1, is connected and composed successively by three cover rectifier units, is respectively the first rectifier unit, the second rectifier unit and the 3rd rectifier unit.First rectifier unit comprises the first head tank 11, first feedstock pump 12, first rectifying tower 13, first condenser 14, first vacuum system 15, first return tank 16, first products pot 17, first reflux pump 18, first product pump 19, first reboiler 110 and the first still material pump 111.First head tank 11, first feedstock pump 12 is connected successively with the first rectifying tower 13.The pneumatic outlet of the first rectifying tower 13 tower top is connected with the input terminus of the first condenser 14, and the fluid output port of the first condenser 14 is then connected with the first return tank 16, and gas enters the first return tank 16 be condensed into liquid in the first condenser 14 after.First vacuum system 15 is connected with the first return tank 16 top.First return tank 16 output terminal establishes two branch roads, wherein a branch road is connected with the first rectifying tower 13 by the first reflux pump 18, partially liq in first return tank 16 is recycled in the first rectifying tower 13, another branch road is connected with the first products pot 17 by the first product pump 19, another part liquid is delivered to the first products pot 17.First reboiler 110 is arranged at the bottom of the tower of the first rectifying tower 13, to heating material vaporization in tower reactor.First still material pump 111 opening for feed is connected with the discharge port of the first rectifying tower 13 bottom discharge mouth and the first reboiler 110.
Second rectifier unit comprises the second charging stock tank 21, second fresh feed pump 22, Second distillation column 23, second condenser 24, second vacuum system 25, second return tank 26, second products pot 27, second reflux pump 28, second product pump 29, second reboiler 210 and the second still material pump 211.Second charging stock tank 21, second fresh feed pump 22 is connected successively with Second distillation column 23.The pneumatic outlet of Second distillation column 23 tower top is connected with the input terminus of the second condenser 24, and the fluid output port of the second condenser 24 is then connected with the second return tank 26, and gas enters the second return tank 26 be condensed into liquid in the second condenser 24 after.Second vacuum system 25 is connected with the second return tank 26 top.Second return tank 26 output terminal establishes two branch roads, wherein a branch road is connected with Second distillation column 23 tower top by the second reflux pump 28, partially liq in second return tank 26 is recycled in Second distillation column 23, another branch road is connected with the second products pot 27 by the second product pump 29, another part liquid is delivered to the second products pot 27.Second reboiler 210 is arranged at the bottom of the tower of Second distillation column 23, to heating material vaporization in tower reactor.Second still material pump 211 opening for feed is connected with the discharge port of Second distillation column 23 bottom discharge mouth and the second reboiler 210.
3rd rectifier unit comprises the 3rd charging stock tank 31, the 3rd fresh feed pump 32, the 3rd rectifying tower 33, the 3rd condenser 34, the 3rd vacuum system 35, the 3rd return tank 36, three products tank 37, the 3rd reflux pump 38, three products pump 39, the 3rd reboiler 310, the 3rd still material pump 311 and still batch can 312.3rd charging stock tank 31, the 3rd fresh feed pump 32 are connected successively with the 3rd rectifying tower 33.The pneumatic outlet of the 3rd rectifying tower 33 tower top is connected with the input terminus of the 3rd condenser 34, and the fluid output port of the 3rd condenser 34 is then connected with the 3rd return tank 36, and gas enters the 3rd return tank 36 be condensed into liquid in the 3rd condenser 34 after.3rd vacuum system 35 is connected with the 3rd return tank 36 top.3rd return tank 36 output terminal establishes two branch roads, wherein a branch road is connected with the 3rd rectifying tower 33 tower top by the 3rd reflux pump 38, partially liq in 3rd return tank 36 is recycled in the 3rd rectifying tower 33, another branch road is connected with three products tank 37 by three products pump 39, and another part liquid is delivered to three products tank 37.3rd reboiler 310 is arranged at the bottom of the tower of the 3rd rectifying tower 33, to heating material vaporization in tower reactor.3rd still material pump 311 opening for feed is connected with the discharge port of the 3rd rectifying tower 33 bottom discharge mouth and the 3rd reboiler 310, and its discharge port is connected with still batch can 312.
First still material pump 111 of the first rectifier unit is connected with the second charging stock tank 21 of the second rectifier unit, and the second still material pump 211 of the second rectifier unit is connected with the 3rd charging stock tank 31 of the 3rd rectifier unit.
technical process:pending desulfurization of raw material alcohol waste liquid puts into the head tank 11 of the first rectifier unit, the first rectifying tower 13 is sent to by the first feedstock pump 12, after the rectifying separation of the first rectifying tower 13, Methyl disulfide in mercaptan removal waste liquid is sent with the tower top of gaseous phase from the first rectifying tower 13, after the first condenser 14 is condensed into liquid, enter the first return tank 16.Liquid in first return tank 16 is divided into two-way, and route first product pump 19 sends the first products pot 17 to, becomes Methyl disulfide product.Another route first reflux pump 18 sends the first rectifying tower 13 back to, to maintain the normal operation of the first rectifying tower 13, after the rectifying separation of the first rectifying tower 13, other components in waste material enter the tower reactor of the first rectifying tower 13 with liquid phase form, are heated by the first reboiler 110, and part still liquid is gasified, reenter bottom the first rectifying tower 13, to maintain the normal operation of the first rectifying tower 13, unnecessary part sends the second charging stock tank 21 to, as the raw material of Second distillation column 23 by the first still material pump 111.Material in second charging stock tank 21 sends Second distillation column 23 to by the second fresh feed pump 22, after the rectifying separation of Second distillation column 23, methylethyl two sulphur in material is sent with the tower top of gaseous phase from Second distillation column 23, after the second condenser 24 is condensed into liquid, enters the second return tank 26.Liquid in second return tank 26 is divided into two-way, and route second product pump 29 sends the second products pot 27 to, becomes methylethyl two sulphur product.Another route second reflux pump 28 sends Second distillation column 23 back to, to maintain the normal operation of rectifying tower, after the rectifying separation of Second distillation column 23, other components in charging enter the tower reactor of Second distillation column 23 with liquid phase form, heated by reboiler, and part still liquid is gasified, reenter bottom Second distillation column 23, to maintain the normal operation of rectifying tower, unnecessary part sends the 3rd charging stock tank 31 to, as the raw material of the 3rd rectifying tower 33 by the second still material pump 211.Material in 3rd charging stock tank 31 sends the 3rd rectifying tower 33 to by the 3rd fresh feed pump 32, after the rectifying separation of the 3rd rectifying tower 33, diethyl two sulphur in material is sent with the tower top of gaseous phase from the 3rd rectifying tower 33, after the 3rd condenser 34 is condensed into liquid, enters the 3rd return tank 36.Liquid in 3rd return tank 36 is divided into two-way, and three products tank 37 sent to by a route three products pump 39, becomes diethyl two sulphur product.Another route the 3rd reflux pump 38 sends the 3rd rectifying tower 33 back to, to maintain the normal operation of the 3rd rectifying tower 33, after the rectifying separation of the 3rd rectifying tower 33, other components in material enter the tower reactor of the 3rd rectifying tower 33 with liquid phase form, are heated by reboiler 310, and part still liquid is gasified, reenter bottom the 3rd rectifying tower 33, to maintain the normal operation of rectifying tower, unnecessary part sends still batch can 312 to by the 3rd still material pump 311, makes waste disposal.
embodiment one:
Employing consists of Methyl disulfide: 44.9%, methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% makes raw material, and start production sequence, Controlling Technology parameter is:
First rectifying tower 13 rectifying section theoretical plate number: 24 pieces, first rectifying tower 13 stripping section theoretical plate number: 26 pieces, first rectifying tower 13 working pressure: normal pressure, first rectifying tower 13 operating reflux ratio: 12 ﹕ 1, first rectifying tower 13 head temperature: 109 DEG C, first rectifying tower 13 opening for feed gas phase temperature: 121 DEG C, the first rectifying tower 13 bottom temperature: 141 DEG C.
Second distillation column 23 rectifying section theoretical plate number: 24 pieces, Second distillation column 23 stripping section theoretical plate number: 26 pieces, 0.02Mpa(is absolute for Second distillation column 23 working pressure), Second distillation column 23 operating reflux ratio: 10 ﹕ 1, Second distillation column 23 head temperature: 101 DEG C, Second distillation column 23 opening for feed gas phase temperature: 108 DEG C, Second distillation column 23 bottom temperature: 126 DEG C.
3rd rectifying tower 33 rectifying section theoretical plate number: 15 pieces, 3rd rectifying tower 33 stripping section theoretical plate number: 15 pieces, 3rd rectifying tower 33 working pressure: 0.02Mpa(is absolute), 3rd rectifying tower 33 operating reflux ratio: 6 ﹕ 1,3rd rectifying tower 33 head temperature: 124 DEG C, 3rd rectifying tower 33 opening for feed gas phase temperature: 127 DEG C, the 3rd rectifying tower 33 bottom temperature: 134 DEG C.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.4%.Methylethyl two sulphur product 40.1%.Diethyl two sulphur product 12.7%.Waste material 1.8%.
embodiment two:
Employing consists of Methyl disulfide: 44.9%, methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% makes raw material, and start production sequence, Controlling Technology parameter is:
First rectifying tower 13 rectifying section theoretical plate number: 24 pieces, first rectifying tower 13 stripping section theoretical plate number: 26 pieces, first rectifying tower 13 working pressure: normal pressure, first rectifying tower 13 operating reflux ratio: 12 ﹕ 1, first rectifying tower 13 head temperature: 109 DEG C, first rectifying tower 13 opening for feed gas phase temperature: 121 DEG C, the first rectifying tower 13 bottom temperature: 141 DEG C.
Second distillation column 23 rectifying section theoretical plate number: 24 pieces, Second distillation column 23 stripping section theoretical plate number: 26 pieces, 0.04Mpa(is absolute for Second distillation column 23 working pressure), Second distillation column 23 operating reflux ratio: 10 ﹕ 1, Second distillation column 23 head temperature: 113 DEG C, Second distillation column 23 opening for feed gas phase temperature: 121 DEG C, Second distillation column 23 bottom temperature: 140 DEG C.
3rd rectifying tower 33 rectifying section theoretical plate number: 15 pieces, 3rd rectifying tower 33 stripping section theoretical plate number: 15 pieces, 3rd rectifying tower 33 working pressure: 0.02Mpa(is absolute), 3rd rectifying tower 33 operating reflux ratio: 6 ﹕ 1,3rd rectifying tower 33 head temperature: 124 DEG C, 3rd rectifying tower 33 opening for feed gas phase temperature: 127 DEG C, the 3rd rectifying tower 33 bottom temperature: 134 DEG C.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.4%.Methylethyl two sulphur product 40.2%.Diethyl two sulphur product 12.7%.Waste material 1.7%.
embodiment three:
Employing consists of Methyl disulfide: 44.9%, methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% makes raw material, and start production sequence, Controlling Technology parameter is:
First rectifying tower 13 rectifying section theoretical plate number: 28 pieces, first rectifying tower 13 stripping section theoretical plate number: 26 pieces, first rectifying tower 13 working pressure: normal pressure, first rectifying tower 13 operating reflux ratio: 12 ﹕ 1, first rectifying tower 13 head temperature: 109 DEG C, first rectifying tower 13 opening for feed gas phase temperature: 120 DEG C, the first rectifying tower 13 bottom temperature: 141 DEG C.
Second distillation column 23 rectifying section theoretical plate number: 28 pieces, Second distillation column 23 stripping section theoretical plate number: 26 pieces, 0.02Mpa(is absolute for Second distillation column 23 working pressure), Second distillation column 23 operating reflux ratio: 10 ﹕ 1, Second distillation column 23 head temperature: 101 DEG C, Second distillation column 23 opening for feed gas phase temperature: 109 DEG C, Second distillation column 23 bottom temperature: 126 DEG C.
3rd rectifying tower 33 rectifying section theoretical plate number: 15 pieces, 3rd rectifying tower 33 stripping section theoretical plate number: 15 pieces, 3rd rectifying tower 33 working pressure: 0.02Mpa(is absolute), 3rd rectifying tower 33 operating reflux ratio: 6 ﹕ 1,3rd rectifying tower 33 head temperature: 124 DEG C, 3rd rectifying tower 33 opening for feed gas phase temperature: 131 DEG C, the 3rd rectifying tower 33 bottom temperature: 136 DEG C.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.3%.Methylethyl two sulphur product 40.2%.Diethyl two sulphur product 13.4%.Waste material 1.1%.
embodiment four:
Employing consists of Methyl disulfide: 44.9%, methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% makes raw material, and start production sequence, Controlling Technology parameter is:
First rectifying tower 13 rectifying section theoretical plate number: 28 pieces, first rectifying tower 13 stripping section theoretical plate number: 26 pieces, first rectifying tower 13 working pressure: normal pressure, first rectifying tower 13 operating reflux ratio: 15 ﹕ 1, first rectifying tower 13 head temperature: 109 DEG C, first rectifying tower 13 opening for feed gas phase temperature: 122 DEG C, the first rectifying tower 13 bottom temperature: 141 DEG C.
Second distillation column 23 rectifying section theoretical plate number: 28 pieces, Second distillation column 23 stripping section theoretical plate number: 26 pieces, 0.02Mpa(is absolute for Second distillation column 23 working pressure), Second distillation column 23 operating reflux ratio: 15 ﹕ 1, Second distillation column 23 head temperature: 101 DEG C, Second distillation column 23 opening for feed gas phase temperature: 107 DEG C, Second distillation column 23 bottom temperature: 126 DEG C.
3rd rectifying tower 33 rectifying section theoretical plate number: 15 pieces, 3rd rectifying tower 33 stripping section theoretical plate number: 15 pieces, 3rd rectifying tower 33 working pressure: 0.02Mpa(is absolute), 3rd rectifying tower 33 operating reflux ratio: 10 ﹕ 1,3rd rectifying tower 33 head temperature: 124 DEG C, 3rd rectifying tower 33 opening for feed gas phase temperature: 130 DEG C, the 3rd rectifying tower 33 bottom temperature: 135 DEG C.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.6%.Methylethyl two sulphur product 39.9%.Diethyl two sulphur product 13.2%.Waste material 1.3%.
embodiment five:
Employing consists of Methyl disulfide: 44.9%, methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% makes raw material, and start production sequence, Controlling Technology parameter is:
First rectifying tower 13 rectifying section theoretical plate number: 24 pieces, first rectifying tower 13 stripping section theoretical plate number: 26 pieces, first rectifying tower 13 working pressure: normal pressure, first rectifying tower 13 operating reflux ratio: 17 ﹕ 1, first rectifying tower 13 head temperature: 109 DEG C, first rectifying tower 13 opening for feed gas phase temperature: 121 DEG C, the first rectifying tower 13 bottom temperature: 141 DEG C.
Second distillation column 23 rectifying section theoretical plate number: 24 pieces, Second distillation column 23 stripping section theoretical plate number: 26 pieces, 0.02Mpa(is absolute for Second distillation column 23 working pressure), Second distillation column 23 operating reflux ratio: 15 ﹕ 1, Second distillation column 23 head temperature: 101 DEG C, Second distillation column 23 opening for feed gas phase temperature: 108 DEG C, Second distillation column 23 bottom temperature: 126 DEG C.
3rd rectifying tower 33 rectifying section theoretical plate number: 20 pieces, 3rd rectifying tower 33 stripping section theoretical plate number: 15 pieces, 3rd rectifying tower 33 working pressure: 0.02Mpa(is absolute), 3rd rectifying tower 33 operating reflux ratio: 8 ﹕ 1,3rd rectifying tower 33 head temperature: 124 DEG C, 3rd rectifying tower 33 opening for feed gas phase temperature: 128 DEG C, the 3rd rectifying tower 33 bottom temperature: 136 DEG C.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.4%.Methylethyl two sulphur product 40.0%.Diethyl two sulphur product 13.4%.Waste material 1.2%.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.The above embodiment of the present invention all can only be thought explanation of the present invention instead of restriction, every above embodiment is done according to substantial technological of the present invention any trickle amendment, equivalent variations and modification, all belong in the scope of technical solution of the present invention.
Claims (1)
1. one kind is continuously separated the technique of pure compound from refinery's mercaptan removal waste liquid, it is characterized in that, mercaptan removal waste liquid is sent to the first rectifier unit rectifying, after Methyl disulfide is separated, liquid at the bottom of the tower of the first rectifier unit is continued to send the second rectifier unit rectifying to, after methylethyl two sulphur is separated, send liquid at the bottom of the tower of the second rectifier unit to the 3rd rectifier unit rectifying, be separated diethyl two sulphur; Wherein, the rectifying condition of described first rectifier unit is: the first rectifying tower rectifying section theoretical plate number: 23-28 block, first rectifying tower stripping section theoretical plate number: 25 ~ 30 pieces, first rectifying tower operation absolute pressure: 0.08 ~ 0.12Mpa, first rectifying tower operating reflux ratio: 12 ~ 17 ﹕ 1, first rectifying tower head temperature: 100 ~ 115 DEG C, the first rectifying tower opening for feed gas phase temperature: 105 ~ 130 DEG C, the first tower bottom of rectifying tower temperature: 125 ~ 145 DEG C; The rectifying condition of described second rectifier unit is: Second distillation column rectifying section theoretical plate number: 23-28 block, Second distillation column stripping section theoretical plate number: 25 ~ 30 pieces, Second distillation column operation absolute pressure 0.02 ~ 0.04 Mpa, Second distillation column operating reflux ratio: 10 ~ 15 ﹕ 1, Second distillation column head temperature: 100 ~ 120 DEG C, Second distillation column opening for feed gas phase temperature: 105 ~ 135 DEG C, Second distillation column bottom temperature: 120 ~ 145 DEG C; The rectifying condition of described 3rd rectifier unit is: the 3rd rectifying tower rectifying section theoretical plate number: 15-20 block, 3rd rectifying tower stripping section theoretical plate number: 15 ~ 20 pieces, 3rd rectifying tower operation absolute pressure: 0.01 ~ 0.03Mpa, 3rd rectifying tower operating reflux ratio: 6 ~ 10:1,3rd rectifying tower head temperature: 110 ~ 130 DEG C, 3rd rectifying tower opening for feed gas phase temperature: 112 ~ 135 DEG C, the 3rd tower bottom of rectifying tower temperature: 120 ~ 145 DEG C.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102950034A (en) * | 2012-10-19 | 2013-03-06 | 中国石油化工股份有限公司 | Vulcanizing agent prepared from sweetening waste liquid secondarily produced from regenerating process of alkali liquor |
| CN102964281A (en) * | 2012-10-19 | 2013-03-13 | 中国石油化工股份有限公司 | Technology and system for preparing vulcanizing agent by using sweetening waste of lye regenerated byproducts |
-
2013
- 2013-10-23 CN CN201310501523.XA patent/CN103539711B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102950034A (en) * | 2012-10-19 | 2013-03-06 | 中国石油化工股份有限公司 | Vulcanizing agent prepared from sweetening waste liquid secondarily produced from regenerating process of alkali liquor |
| CN102964281A (en) * | 2012-10-19 | 2013-03-13 | 中国石油化工股份有限公司 | Technology and system for preparing vulcanizing agent by using sweetening waste of lye regenerated byproducts |
Non-Patent Citations (1)
| Title |
|---|
| 液化气脱硫醇装置碱渣减排的探索及实践;余伟等;《工业安全与环保》;20120331;第38卷(第3期);78-81 * |
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| CN103539711A (en) | 2014-01-29 |
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