CN103788126B - A kind of ethrel continuous acidolysis method - Google Patents
A kind of ethrel continuous acidolysis method Download PDFInfo
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- CN103788126B CN103788126B CN201410012251.1A CN201410012251A CN103788126B CN 103788126 B CN103788126 B CN 103788126B CN 201410012251 A CN201410012251 A CN 201410012251A CN 103788126 B CN103788126 B CN 103788126B
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Abstract
The invention discloses a kind of ethrel continuous acidolysis method, adopt n level ladder autoclave successive reaction, 2-chloroethyl di(2-ethylhexyl)phosphate (2-chloroethyl) ester enters acidolysis the 1st order reaction still, material enters next stage reactor from the extraction of upper level Polycondensation Reactor and Esterification Reactor, until enter the n-th order reaction still A, switching from the material of extraction at the bottom of the (n-1)th order reaction still still when material in the n-th order reaction still A reaches 4/5 volume enters the n-th order reaction still B, n-th grade of still A continues logical hydrogenchloride insulation, discharging after insulation 4h, the material of 1/10 volume is retained in n-th order reaction still A at the end of discharging, switching from the material of extraction at the bottom of the (n-1)th order reaction still still when material in the n-th order reaction still B reaches 4/5 volume enters the n-th order reaction still A, cyclical operation successively, hydrogenchloride is passed into by the bottom of reactor at different levels, unreacted hydrogenchloride is reclaimed through compressor recycle after being cooled by top, the integer of n value 2 ~ 10.
Description
Technical field
The present invention relates to the preparation method of ethrel, be specifically related to ethrel continuous acidolysis method, belong to technical field of chemical engineering.
Background technology
Conventional ethylene profit acidolysis process is produced, main employing batch tank method.This method, add phase hydrogenchloride consumption in acidolysis reaction early stage and diester large, the full-load operation of hydrogenchloride make up compressor still can not be satisfied the demand, and phase after the reaction, consumes hydrogenchloride hardly, and hydrogenchloride make up compressor must backflow, makes idle work.The instability of hydrogenchloride consumption causes system pressure big rise and fall simultaneously, thus the infringement of aggravation equipment, pipeline.
Acidolysis reaction is divided into two-stage, first order reaction heat release, and second order reaction is absorbed heat.Existing device adopts batch tank reaction, adopts cold and hot oils alternation to use and controls temperature of reaction, cause energy dissipation larger.
The stable coordination of each workshop section of hydrogenchloride spending rate influence of fluctuations that batch production causes, particularly with being connected of resolving hydrochloric acid, that synthesizes with hydrochloric acid is connected, and that packs with allotment is connected.Greatly often, occur that resolving hydrochloric acid does not catch up with, hydrogenchloride consumption hour there will be again the situations such as resolving hydrochloric acid ability surplus at hydrogenchloride consumption, exacerbate the not easy operation control simultaneously of Analytic Tower burden.
Each operation order of classes or grades at school causes discharging batch too concentrated sometimes because objective and subjective reason causes, allotment, chemical examination ability such as not to catch up with at the contradiction.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of ethrel continuous acidolysis method, to solve during traditional batch autoclave is produced the series of problems such as energy waste, maintenance of the equipment, production coordination occurred.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of ethrel continuous acidolysis method, adopt n level ladder autoclave successive reaction, 2-chloroethyl di(2-ethylhexyl)phosphate (2-chloroethyl) ester enters acidolysis the 1st order reaction still, material enters next stage reactor from the extraction of upper level Polycondensation Reactor and Esterification Reactor, until enter the n-th order reaction still A, switching from the material of extraction at the bottom of the (n-1)th order reaction still still when material in the n-th order reaction still A reaches 4/5 volume enters the n-th order reaction still B, n-th grade of still A continues logical hydrogenchloride insulation, discharging after insulation 4h, the material retaining 1/10 volume at the end of discharging in n-th order reaction still A (prevents hydrogenchloride in three grades of still A from entering exhaust system from discharge nozzle through compounding kettle, reduce hydrogenchloride quantity discharged), switching from the material of extraction at the bottom of the (n-1)th order reaction still still when material in the n-th order reaction still B reaches 4/5 volume enters the n-th order reaction still A, cyclical operation successively, hydrogenchloride is passed into by the bottom of reactor at different levels, unreacted hydrogenchloride is reclaimed through compressor recycle after being cooled by top, the integer of n value 2 ~ 10, n preferably 3.
Wherein, described reactor is enamel still, chemical reaction still, the tower reactor of graphite or tubular reactor.
Wherein, the volume of the reactor described in reactor is 500-50000L, and the use volume of reactor is 1/2 ~ 4/5 volume.
Wherein, the 1st order reaction still temperature in the kettle is 100-180 DEG C, and pressure is 0.3-0.5MPa; 2nd ~ n order reaction temperature in the kettle is lower 10 DEG C than the 1st order reaction still temperature, and pressure is 0.3-0.5MPa.
Reaction was violent, and ethylene dichloride gas concentrates extraction to cause material parts to carry secretly, needs cold oil cool between the reaction period 1-5 hour period early stage for the reaction of 1st grade of still, and two, third order reaction is comparatively steady, appropriateness is incubated.
Beneficial effect: the present invention adopts staged continuous acidolysis process method, effectively can solve during traditional batch autoclave is produced the series of problems such as energy waste, maintenance of the equipment, production coordination occurred, be beneficial to control, be convenient to produce, reduce energy loss, increase enterprise profit.
1. ethrel content promotes one percentage point on the original basis;
2. the acidolysis recycle system is more stable, and daily checking maintenance amount reduces;
3. energy waste reduces;
4. production efficiency increases, and staff labor intensity reduces.
Accompanying drawing explanation
Fig. 1 is device of the present invention and schematic flow sheet.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
Embodiment 1:
Adopt three grades of ladder autoclave successive reactions (as Fig. 1), 2-chloroethyl di(2-ethylhexyl)phosphate (2-chloroethyl) ester enters acidolysis one-level still (volume 8000L), at the bottom of still, extraction enters secondary still (volume 8000L), again from extraction three grades of still A(volume 10000L at the bottom of secondary still still), when in three grades of still A, material reaches 8000L, switch to three grades of still B(volume 10000L), three grades of still A continue logical hydrogenchloride insulation, discharging after insulation 4h, retaining 1000L material at the end of discharging in still (prevents hydrogenchloride in three grades of still A from entering exhaust system from discharge nozzle through compounding kettle, reduce hydrogenchloride quantity discharged), three grades of still A are switched to when material reaches 8000L in three grades of still B, cyclical operation successively.Hydrogenchloride is passed into by the bottom of reactor at different levels, reclaims unreacted hydrogenchloride through compressor recycle by top after being cooled.
Aforesaid reaction vessel is pressurized vessel, comprises enamel still, chemical reaction still, the tower reactor of graphite, tubular reactor etc.
One-level still temperature in the kettle described in above-mentioned technique is at 150 DEG C, and pressure maintains 0.4MPa.Secondary, three grades of still temperature in the kettle are low relative to one-level still temperature in the kettle about 10 DEG C.
10,000 tons of ethrels (folding 100%) are produced per year according to current device, 4 acidolysis still yearly capacities are 5000 tons of ethrels (foldings 100%), working time in device year calculated by 300 days, and continuous acidolysis 2-chloroethyl di(2-ethylhexyl)phosphate (2-chloroethyl) ester feed rate is: 5000 × 2 × 1000 ÷ 300 ÷ 24=1390kg/h.
First order reaction still, second order reaction still design volume is 8000L, third order reaction still design volume is 10000L, use volume to be 5000L according to first order reaction still, second order reaction still, third order reaction still is that 8000L calculates the residence time: (5000+5000+8000+8000) × 1.3 ÷ 1390 × 2=48.6h.Current intermittent type acidolysis reaction cycle 40 ~ 45h, the residence time is greater than current reaction time.
Existing rhythmic reaction device can not realize continuous prodution.
Claims (3)
1. an ethrel continuous acidolysis method, it is characterized in that, adopt n level ladder autoclave successive reaction, 2-chloroethyl di(2-ethylhexyl)phosphate (2-chloroethyl) ester enters acidolysis the 1st order reaction still, material enters next stage reactor from the extraction of upper level Polycondensation Reactor and Esterification Reactor, until enter the n-th order reaction still A, switching from the material of extraction at the bottom of the (n-1)th order reaction still still when material in the n-th order reaction still A reaches 4/5 volume enters the n-th order reaction still B, n-th grade of still A continues logical hydrogenchloride insulation, discharging after insulation 4h, the material of 1/10 volume is retained in n-th order reaction still A at the end of discharging, switching from the material of extraction at the bottom of the (n-1)th order reaction still still when material in the n-th order reaction still B reaches 4/5 volume enters the n-th order reaction still A, cyclical operation successively, hydrogenchloride is passed into by the bottom of reactor at different levels, unreacted hydrogenchloride is reclaimed through compressor recycle after being cooled by top, the integer of n value 2 ~ 3,
1st order reaction still temperature in the kettle is 100-180 DEG C, and pressure is 0.3-0.5MPa; 2nd ~ n order reaction temperature in the kettle is lower 10 DEG C than the 1st order reaction still temperature, and pressure is 0.3-0.5MPa.
2. ethrel continuous acidolysis method according to claim 1, is characterized in that, described reactor is enamel still, chemical reaction still, the tower reactor of graphite or tubular reactor.
3. ethrel continuous acidolysis method according to claim 1, is characterized in that, the volume of described reactor is 500-50000L, and the use volume of reactor is 1/2 ~ 4/5 volume.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD266933A3 (en) * | 1986-07-28 | 1989-04-19 | Bitterfeld Chemie | PROCESS FOR PREPARING 2-CHLOROETHANOPHOSPHONIC ACID |
| CN1048043A (en) * | 1989-06-14 | 1990-12-26 | 上海市农药研究所 | The preparation method of 2 chloroethyl phosphoric acid |
| CN1253952A (en) * | 1999-10-08 | 2000-05-24 | 常熟市农药厂 | Preparation method of 70%-80% liquid 2-chloroethyl phosphonic acid |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD258237A5 (en) * | 1985-10-18 | 1988-07-13 | ��K@�����`�������@����������k�� | PROCESS FOR PREPARING AN ALIPHATIC PHOSPHONIC ACID |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DD266933A3 (en) * | 1986-07-28 | 1989-04-19 | Bitterfeld Chemie | PROCESS FOR PREPARING 2-CHLOROETHANOPHOSPHONIC ACID |
| CN1048043A (en) * | 1989-06-14 | 1990-12-26 | 上海市农药研究所 | The preparation method of 2 chloroethyl phosphoric acid |
| CN1253952A (en) * | 1999-10-08 | 2000-05-24 | 常熟市农药厂 | Preparation method of 70%-80% liquid 2-chloroethyl phosphonic acid |
Non-Patent Citations (1)
| Title |
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| 孙德群 等.乙烯利加压法合成工艺改进.《现代农药》.2008,第7卷(第6期),19-21. * |
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Address after: 223002 No. 30, Chemical Road, Huaian, Jiangsu Patentee after: Andao mai'anbang (Jiangsu) Co., Ltd Address before: 223002 No. 30, Chemical Road, Huaian, Jiangsu Patentee before: JIANGSU ANPON ELECTROCHEMICAL Co.,Ltd. |
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