CN103539711A - Technology for continuously separating pure compounds from mercaptan removal waste liquid in refinery plant - Google Patents
Technology for continuously separating pure compounds from mercaptan removal waste liquid in refinery plant Download PDFInfo
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Abstract
The invention discloses a technology for continuously separating pure compounds from mercaptan removal waste liquid in a refinery plant. The technology is characterized in that mercaptan removal waste liquid is fed into a first rectification device so as to be rectified, after dimethyl disulfide is separated out, the tower bottom liquid of the first rectification device is continuously fed into a second rectification device so as to be rectified, after methyl ethyl disulfide is separated out, and the tower bottom liquid of the second rectification device is continuously fed into a third rectification device so as to be rectified, so that diethyl disulfide is separated out. The technology has the advantages that the pure compound components are separated from the mercaptan removal waste liquid, the dimethyl disulfide, methyl ethyl disulfide and diethyl disulfide products which are separated out respectively reach above 99% and meet the quality requirements of the pure compounds, and the yield of the produced products reaches above 95%.
Description
Technical field
The present invention relates to the technique of separating compound, relate in particular to a kind of from refinery's mercaptan removal waste liquid continuous separate from the technique of pure compound.
Background technology
The liquefied petroleum gas (LPG) that refinery is produced all needs to process through mercaptan removal before dispatching from the factory, and treatment process is for contacting with liquefied gas with alkali lye.Mercaptan in liquefied gas reacts generation sodium mercaptides with the NaOH in alkali lye, the sodium mercaptides generating is dissolved in alkali lye, realize removing of mercaptan in liquefied gas, in doctor process in early days, after NaOH in alkali lye consumes completely, alkali lye is conveyed to wastewater treatment equipment and processes, and causes cost for wastewater treatment very large.In recent years, Ningbo Zhong Yi company has developed alkali lye oxygen-rich oxide regeneration techniques, and many refinery application at home, and the oxygen rich air that this technology utilizes refinery air separation facility to produce is carried 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 is immiscible, after stratification, and separated alkali lye, realizes alkali liquid regeneration and recycle.The waste liquid of separating is mercaptan removal waste liquid, and its main component is disulphide.Because disulphide is a kind of violent in toxicity of high sulfur-bearing, as be dispersed in environment, can cause severe contamination, therefore need do special processing, destroy its molecular structure to eliminate or reduction 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 costss, and burning process produces a large amount of sulfurous gas, still environment is produced to serious pollution, fails thoroughly to solve the pollution to environment.
The technique of 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 good mercaptan removal waste water utilization method, but the product application face of gained is narrower, absorption of market is limited, and can not complete digestion refinery production process producing is mercaptan removal waste liquid, and a large amount of mercaptan removal waste liquids still awaits developing.
Summary of the invention
The object of this invention is to provide from refinery's mercaptan removal waste liquid continuous separate from the technique of pure compound, this technique can continuous separate from 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 from refinery's mercaptan removal waste liquid continuous separate from the technique of pure compound, send mercaptan removal waste liquid to 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 to the second rectifier unit rectifying, after methylethyl two sulphur are separated, send liquid at the bottom of the tower of the second rectifier unit to the 3rd rectifier unit rectifying, separated diethyl two sulphur.
In mercaptan removal waste liquid, contain following compound: Methyl disulfide, methylethyl two sulphur, dimethyltrisulfide, diethyl two sulphur and on a small quantity other sulfide, simultaneously with high-boiling-point impurities such as micro-sodium hydroxide, semi-annular jade pendant phthalein cyanogen cobalts, be summed up as metallic compound and the large class of nonmetallic compound two, the boiling spread of nonmetallic compound is between 108 ℃ ~ 165 ℃, and the boiling point of metallic compound is more than 300 ℃.The boiling point of Methyl disulfide is 109 ℃, and the boiling point of methylethyl two sulphur is 131 ℃, and the boiling point of diethyl two sulphur is 154 ℃, and the boiling point of dimethyltrisulfide, for being greater than 170 ℃, can adopt the method for fractionation to carry out separation to the pure compound in mercaptan removal waste liquid.In the present invention, adopt three rectifier units to carry out separated to Methyl disulfide, methylethyl two sulphur, diethyl two sulphur with dimethyltrisulfide, in each concrete distillation operation, according to operating features separately, can select tower top temperature, tower reactor temperature, interior certain some temperature of tower as main control parameters.In the present invention's the first rectifying tower, owing to requiring overhead product Methyl disulfide purity more than 99%, require the Methyl disulfide content of tower kettle product below 0.5% simultaneously, but in operating process, when the purity of overhead product occurs slightly to change, the reaction of tower top temperature is not obvious, can not operate control according to tower top temperature, and when changing appears in the ratio of methylethyl two sulphur and diethyl two sulphur, in normal running, tower reactor temperature there will be variation, therefore can not operate control according to tower reactor temperature.And when subtle change appears in overhead product purity, opening for feed vapor phase temperature has compared with considerable change, and methylethyl two sulphur of raw material and the variation of diethyl two sulphur ratios are little on the impact of opening for feed vapor phase temperature, control opening for feed vapor phase temperature higher than tower top temperature certain limit, can reach the separate targets of the first rectifying tower, thereby select opening for feed vapor phase temperature to control parameter as the main operation 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.The 3rd rectifying tower selects tower reactor temperature as main control parameters, the object of the 3rd rectifying tower is to obtain the satisfactory overhead product of purity, tower kettle product is as waste disposal, control tower reactor temperature higher than tower top temperature certain limit, can guarantee the purity of overhead product, also guarantee 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 operating process, are also noted that the tower reactor 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 piece, rectifying tower stripping section theoretical plate number: 25-30 piece, rectifying tower operation absolute pressure: 0.08-0.12Mpa, rectifying tower operating reflux ratio: 12-17 ﹕ 1, rectifying tower top temperature: 100-115 ℃, rectifying tower opening for feed gas phase temperature: 105-130 ℃, tower bottom of rectifying tower temperature: 125-145 ℃.
The rectifying condition optimization of the second rectifier unit of the present invention is: rectifying tower rectifying section theoretical plate number: 23-28 piece, rectifying tower stripping section theoretical plate number: 25-30 piece, rectifying tower operation absolute pressure 0.02-0.04 Mpa, rectifying tower operating reflux ratio: 10-15 ﹕ 1, rectifying tower top temperature: 100-120 ℃, rectifying tower opening for feed gas phase temperature: 105-135 ℃, tower bottom of rectifying tower temperature: 120-145 ℃.
The rectifying condition optimization of the 3rd rectifier unit of the present invention is: rectifying tower rectifying section theoretical plate number: 15-20 piece, rectifying tower stripping section theoretical plate number: 15-20 piece, rectifying tower operation absolute pressure: 0.01-0.03Mpa, rectifying tower operating reflux ratio: 6-10 ﹕ 1, rectifying tower top temperature: 110-130 ℃, rectifying tower opening for feed gas phase temperature: 112-135 ℃, tower bottom of rectifying tower temperature: 120-145 ℃.
the present invention compared with prior art has the following advantages:
The present invention has realized and from mercaptan removal waste liquid, has isolated pure compound component, the Methyl disulfide of separating, methylethyl two sulphur, diethyl two sulphur product purities reach more than 99%, reach the specification of quality of pure compound, the product yield of production reaches more than 95%, and three kinds of products producing due to the present invention are the huge product of market capacity, greatly widened the application of mercaptan removal waste liquid, the outlet of mercaptan removal waste liquid is solved preferably.The present invention has adopted rational temperature, pressure parameter, does not exist in process of production material to 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 that continuous separate is used from 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.The first rectifier unit comprises the first head tank 11, the first feedstock pump 12, the first rectifying tower 13, the first condenser 14, the first vacuum system 15, the first return tank 16, the first products pot 17, the first reflux pump 18, the first product pump 19, the first reboiler 110 and the first still material pump 111.The first head tank 11, the first feedstock pump 12 are connected successively with the first rectifying tower 13.The pneumatic outlet of the first rectifying tower 13 tower tops is connected with the input terminus of the first condenser 14, and the liquid output terminal of the first condenser 14 is 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.The first vacuum system 15 is connected with the first return tank 16 tops.The first return tank 16 output terminals are established two branch roads, wherein a branch road is connected with the first rectifying tower 13 by the first reflux pump 18, partially liq in the 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, and another part liquid is delivered to the first products pot 17.At the bottom of the first reboiler 110 is arranged on the tower of the first rectifying tower 13, to heating material vaporization in tower reactor.The first still material pump 111 opening for feeds are connected with the discharge port of the first reboiler 110 with the first rectifying tower 13 bottom discharge mouths.
The second rectifier unit comprises the second charging stock tank 21, the second fresh feed pump 22, Second distillation column 23, the second condenser 24, the second vacuum system 25, the second return tank 26, the second products pot 27, the second reflux pump 28, the second product pump 29, the second reboiler 210 and the second still material pump 211.The second charging stock tank 21, the second fresh feed pump 22 are connected successively with Second distillation column 23.The pneumatic outlet of Second distillation column 23 tower tops is connected with the input terminus of the second condenser 24, and the liquid output terminal of the second condenser 24 is 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.The second vacuum system 25 is connected with the second return tank 26 tops.The second return tank 26 output terminals are established two branch roads, wherein a branch road is connected with Second distillation column 23 tower tops by the second reflux pump 28, partially liq in the 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, and another part liquid is delivered to the second products pot 27.At the bottom of the second reboiler 210 is arranged on the tower of Second distillation column 23, to heating material vaporization in tower reactor.The second still material pump 211 opening for feeds are connected with the discharge port of the second reboiler 210 with Second distillation column 23 bottom discharge mouths.
The 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.The 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 tops is connected with the input terminus of the 3rd condenser 34, and the liquid output terminal of the 3rd condenser 34 is 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.The 3rd vacuum system 35 is connected with the 3rd return tank 36 tops.The 3rd return tank 36 output terminals are established two branch roads, wherein a branch road is connected with the 3rd rectifying tower 33 tower tops by the 3rd reflux pump 38, partially liq in the 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.At the bottom of the 3rd reboiler 310 is arranged on the tower of the 3rd rectifying tower 33, to heating material vaporization in tower reactor.The 3rd still material pump 311 opening for feeds are connected with the discharge port of the 3rd reboiler 310 with the 3rd rectifying tower 33 bottom discharge mouths, and its discharge port is connected with still batch can 312.
The 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 is put into the head tank 11 of the first rectifier unit, by the first feedstock pump 12, send the first rectifying tower 13 to, after the rectifying separation of the first rectifying tower 13, Methyl disulfide in mercaptan removal waste liquid is sent from the tower top of the first rectifying tower 13 with gaseous phase, through the first condenser 14, be condensed into after liquid, enter the first return tank 16.Liquid in the first return tank 16 is divided into two-way, and route first product pump 19 is sent the first products pot 17 to, becomes Methyl disulfide product.Another route first reflux pump 18 is sent 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, by the first reboiler 110 heating, make the gasification of part still liquid, reenter the first rectifying tower 13 bottoms, to maintain the normal operation of the first rectifying tower 13, unnecessary part is sent the second charging stock tank 21 to by the first still material pump 111, as the raw material of Second distillation column 23.Material in the second charging stock tank 21 is sent 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 are sent from the tower top of Second distillation column 23 with gaseous phase, through the second condenser 24, are condensed into after liquid, enter the second return tank 26.Liquid in the second return tank 26 is divided into two-way, and route second product pump 29 is sent the second products pot 27 to, becomes methylethyl two sulphur products.Another route second reflux pump 28 is sent 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, by reboiler, heat, and make the gasification of part still liquid, reenter Second distillation column 23 bottoms, to maintain the normal operation of rectifying tower, unnecessary part is sent the 3rd charging stock tank 31 to by the second still material pump 211, as the raw material of the 3rd rectifying tower 33.Material in the 3rd charging stock tank 31 is sent 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 are sent from the tower top of the 3rd rectifying tower 33 with gaseous phase, through the 3rd condenser 34, are condensed into after liquid, enter the 3rd return tank 36.Liquid in the 3rd return tank 36 is divided into two-way, and a route three products pump 39 is sent three products tank 37 to, becomes diethyl two sulphur products.Another route the 3rd reflux pump 38 is sent 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, by reboiler 310, heat, and make the gasification of part still liquid, reenter the 3rd rectifying tower 33 bottoms, to maintain the normal operation of rectifying tower, unnecessary part is sent still batch can 312 to by the 3rd still material pump 311, makes waste disposal.
embodiment mono-:
Employing consists of Methyl disulfide: 44.9%, and methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% is made raw material, starts production sequence, controls processing parameter and is:
The first rectifying tower 13 rectifying section theoretical plate numbers: 24, the first rectifying tower 13 stripping section theoretical plate numbers: 26, the first rectifying tower 13 working pressures: normal pressure, the first rectifying tower 13 operating reflux ratios: 12 ﹕ 1, the first rectifying tower 13 head temperature: 109 ℃, the first rectifying tower 13 opening for feed gas phase temperatures: 121 ℃, the first rectifying tower 13 tower reactor temperature: 141 ℃.
Second distillation column 23 rectifying section theoretical plate numbers: 24, Second distillation column 23 stripping section theoretical plate numbers: 26,23 working pressure 0.02Mpa(are absolute for Second distillation column), Second distillation column 23 operating reflux ratios: 10 ﹕ 1, Second distillation column 23 head temperature: 101 ℃, Second distillation column 23 opening for feed gas phase temperatures: 108 ℃, Second distillation column 23 tower reactor temperature: 126 ℃.
The 3rd rectifying tower 33 rectifying section theoretical plate numbers: 15, the 3rd rectifying tower 33 stripping section theoretical plate numbers: 15, the 3rd rectifying tower 33 working pressures: 0.02Mpa(is absolute), the 3rd rectifying tower 33 operating reflux ratios: 6 ﹕ 1, the 3rd rectifying tower 33 head temperature: 124 ℃, the 3rd rectifying tower 33 opening for feed gas phase temperatures: 127 ℃, the 3rd rectifying tower 33 tower reactor temperature: 134 ℃.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.4%.Methylethyl two sulphur products 40.1%.Diethyl two sulphur products 12.7%.Waste material 1.8%.
embodiment bis-:
Employing consists of Methyl disulfide: 44.9%, and methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% is made raw material, starts production sequence, controls processing parameter and is:
The first rectifying tower 13 rectifying section theoretical plate numbers: 24, the first rectifying tower 13 stripping section theoretical plate numbers: 26, the first rectifying tower 13 working pressures: normal pressure, the first rectifying tower 13 operating reflux ratios: 12 ﹕ 1, the first rectifying tower 13 head temperature: 109 ℃, the first rectifying tower 13 opening for feed gas phase temperatures: 121 ℃, the first rectifying tower 13 tower reactor temperature: 141 ℃.
Second distillation column 23 rectifying section theoretical plate numbers: 24, Second distillation column 23 stripping section theoretical plate numbers: 26,23 working pressure 0.04Mpa(are absolute for Second distillation column), Second distillation column 23 operating reflux ratios: 10 ﹕ 1, Second distillation column 23 head temperature: 113 ℃, Second distillation column 23 opening for feed gas phase temperatures: 121 ℃, Second distillation column 23 tower reactor temperature: 140 ℃.
The 3rd rectifying tower 33 rectifying section theoretical plate numbers: 15, the 3rd rectifying tower 33 stripping section theoretical plate numbers: 15, the 3rd rectifying tower 33 working pressures: 0.02Mpa(is absolute), the 3rd rectifying tower 33 operating reflux ratios: 6 ﹕ 1, the 3rd rectifying tower 33 head temperature: 124 ℃, the 3rd rectifying tower 33 opening for feed gas phase temperatures: 127 ℃, the 3rd rectifying tower 33 tower reactor temperature: 134 ℃.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.4%.Methylethyl two sulphur products 40.2%.Diethyl two sulphur products 12.7%.Waste material 1.7%.
embodiment tri-:
Employing consists of Methyl disulfide: 44.9%, and methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% is made raw material, starts production sequence, controls processing parameter and is:
The first rectifying tower 13 rectifying section theoretical plate numbers: 28, the first rectifying tower 13 stripping section theoretical plate numbers: 26, the first rectifying tower 13 working pressures: normal pressure, the first rectifying tower 13 operating reflux ratios: 12 ﹕ 1, the first rectifying tower 13 head temperature: 109 ℃, the first rectifying tower 13 opening for feed gas phase temperatures: 120 ℃, the first rectifying tower 13 tower reactor temperature: 141 ℃.
Second distillation column 23 rectifying section theoretical plate numbers: 28, Second distillation column 23 stripping section theoretical plate numbers: 26,23 working pressure 0.02Mpa(are absolute for Second distillation column), Second distillation column 23 operating reflux ratios: 10 ﹕ 1, Second distillation column 23 head temperature: 101 ℃, Second distillation column 23 opening for feed gas phase temperatures: 109 ℃, Second distillation column 23 tower reactor temperature: 126 ℃.
The 3rd rectifying tower 33 rectifying section theoretical plate numbers: 15, the 3rd rectifying tower 33 stripping section theoretical plate numbers: 15, the 3rd rectifying tower 33 working pressures: 0.02Mpa(is absolute), the 3rd rectifying tower 33 operating reflux ratios: 6 ﹕ 1, the 3rd rectifying tower 33 head temperature: 124 ℃, the 3rd rectifying tower 33 opening for feed gas phase temperatures: 131 ℃, the 3rd rectifying tower 33 tower reactor temperature: 136 ℃.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.3%.Methylethyl two sulphur products 40.2%.Diethyl two sulphur products 13.4%.Waste material 1.1%.
embodiment tetra-:
Employing consists of Methyl disulfide: 44.9%, and methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% is made raw material, starts production sequence, controls processing parameter and is:
The first rectifying tower 13 rectifying section theoretical plate numbers: 28, the first rectifying tower 13 stripping section theoretical plate numbers: 26, the first rectifying tower 13 working pressures: normal pressure, the first rectifying tower 13 operating reflux ratios: 15 ﹕ 1, the first rectifying tower 13 head temperature: 109 ℃, the first rectifying tower 13 opening for feed gas phase temperatures: 122 ℃, the first rectifying tower 13 tower reactor temperature: 141 ℃.
Second distillation column 23 rectifying section theoretical plate numbers: 28, Second distillation column 23 stripping section theoretical plate numbers: 26,23 working pressure 0.02Mpa(are absolute for Second distillation column), Second distillation column 23 operating reflux ratios: 15 ﹕ 1, Second distillation column 23 head temperature: 101 ℃, Second distillation column 23 opening for feed gas phase temperatures: 107 ℃, Second distillation column 23 tower reactor temperature: 126 ℃.
The 3rd rectifying tower 33 rectifying section theoretical plate numbers: 15, the 3rd rectifying tower 33 stripping section theoretical plate numbers: 15, the 3rd rectifying tower 33 working pressures: 0.02Mpa(is absolute), the 3rd rectifying tower 33 operating reflux ratios: 10 ﹕ 1, the 3rd rectifying tower 33 head temperature: 124 ℃, the 3rd rectifying tower 33 opening for feed gas phase temperatures: 130 ℃, the 3rd rectifying tower 33 tower reactor temperature: 135 ℃.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.6%.Methylethyl two sulphur products 39.9%.Diethyl two sulphur products 13.2%.Waste material 1.3%.
embodiment five:
Employing consists of Methyl disulfide: 44.9%, and methylethyl two sulphur: 40.1%, diethyl two sulphur: 14.5%, dimethyltrisulfide: 0.5%, the mercaptan removal waste liquid of metallic compound: < 0.1% is made raw material, starts production sequence, controls processing parameter and is:
The first rectifying tower 13 rectifying section theoretical plate numbers: 24, the first rectifying tower 13 stripping section theoretical plate numbers: 26, the first rectifying tower 13 working pressures: normal pressure, the first rectifying tower 13 operating reflux ratios: 17 ﹕ 1, the first rectifying tower 13 head temperature: 109 ℃, the first rectifying tower 13 opening for feed gas phase temperatures: 121 ℃, the first rectifying tower 13 tower reactor temperature: 141 ℃.
Second distillation column 23 rectifying section theoretical plate numbers: 24, Second distillation column 23 stripping section theoretical plate numbers: 26,23 working pressure 0.02Mpa(are absolute for Second distillation column), Second distillation column 23 operating reflux ratios: 15 ﹕ 1, Second distillation column 23 head temperature: 101 ℃, Second distillation column 23 opening for feed gas phase temperatures: 108 ℃, Second distillation column 23 tower reactor temperature: 126 ℃.
The 3rd rectifying tower 33 rectifying section theoretical plate numbers: 20, the 3rd rectifying tower 33 stripping section theoretical plate numbers: 15, the 3rd rectifying tower 33 working pressures: 0.02Mpa(is absolute), the 3rd rectifying tower 33 operating reflux ratios: 8 ﹕ 1, the 3rd rectifying tower 33 head temperature: 124 ℃, the 3rd rectifying tower 33 opening for feed gas phase temperatures: 128 ℃, the 3rd rectifying tower 33 tower reactor temperature: 136 ℃.
Products obtained therefrom quality is:
Each product yield is: Methyl disulfide product 45.4%.Methylethyl two sulphur products 40.0%.Diethyl two sulphur products 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 think explanation of the present invention rather than restriction, and any trickle modification, equivalent variations and modification that every foundation essence technology of the present invention is done above embodiment, all belong in the scope of technical solution of the present invention.
Claims (4)
- In 1.Yi Zhongcong refinery mercaptan removal waste liquid, continuous separate is from the technique of pure compound, it is characterized in that, send mercaptan removal waste liquid to 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 to the second rectifier unit rectifying, after methylethyl two sulphur are separated, send liquid at the bottom of the tower of the second rectifier unit to the 3rd rectifier unit rectifying, separated diethyl two sulphur.
- 2. the technique of preparing vulcanizing agent with the mercaptan removal waste liquid of alkali liquid regeneration by-product according to claim 1, it is characterized in that, the rectifying condition of described the first rectifier unit is: the first rectifying tower rectifying section theoretical plate number: 23-28 piece, the first rectifying tower stripping section theoretical plate number: 25 ~ 30, first rectifying tower operation absolute pressure: 0.08 ~ 0.12Mpa, the first rectifying tower operating reflux ratio: 12 ~ 17 ﹕ 1, the first rectifying tower top temperature: 100 ~ 115 ℃, the first rectifying tower opening for feed gas phase temperature: 105 ~ 130 ℃, the first tower bottom of rectifying tower temperature: 125 ~ 145 ℃.
- 3. the technique of preparing vulcanizing agent with the mercaptan removal waste liquid of alkali liquid regeneration by-product according to claim 1, it is characterized in that, the rectifying condition of described the second rectifier unit is: Second distillation column rectifying section theoretical plate number: 23-28 piece, Second distillation column stripping section theoretical plate number: 25 ~ 30, 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 ℃, Second distillation column opening for feed gas phase temperature: 105 ~ 135 ℃, Second distillation column tower reactor temperature: 120 ~ 145 ℃.
- 4. the technique of preparing vulcanizing agent with the mercaptan removal waste liquid of alkali liquid regeneration by-product according to claim 1, it is characterized in that, the rectifying condition of described the 3rd rectifier unit is: the 3rd rectifying tower rectifying section theoretical plate number: 15-20 piece, the 3rd rectifying tower stripping section theoretical plate number: 15 ~ 20, the 3rd rectifying tower operation absolute pressure: 0.01 ~ 0.03Mpa, the 3rd rectifying tower operating reflux ratio: 6 ~ 10:1, the 3rd rectifying tower top temperature: 110 ~ 130 ℃, the 3rd rectifying tower opening for feed gas phase temperature: 112 ~ 135 ℃, the 3rd tower bottom of rectifying tower temperature: 120 ~ 145 ℃.
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| CN103880722A (en) * | 2014-03-31 | 2014-06-25 | 宁波中一石化科技股份有限公司 | Method for preparing high-purity diethyl disulfide |
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| 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 |
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| CN103880722A (en) * | 2014-03-31 | 2014-06-25 | 宁波中一石化科技股份有限公司 | Method for preparing high-purity diethyl disulfide |
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| CN103539711B (en) | 2015-09-16 |
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