CN100590121C - Close-circulating chlorohydrination reactor and reactive method during production of epoxy-propane - Google Patents
Close-circulating chlorohydrination reactor and reactive method during production of epoxy-propane Download PDFInfo
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- CN100590121C CN100590121C CN200710011074A CN200710011074A CN100590121C CN 100590121 C CN100590121 C CN 100590121C CN 200710011074 A CN200710011074 A CN 200710011074A CN 200710011074 A CN200710011074 A CN 200710011074A CN 100590121 C CN100590121 C CN 100590121C
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- Prior art keywords
- propylene
- gas
- pipe
- chlorine
- chlorohydrin
- Prior art date
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- 238000000034 method Methods 0.000 title claims abstract description 19
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- QQONPFPTGQHPMA-UHFFFAOYSA-N Propene Chemical compound CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000007789 gas Substances 0.000 claims abstract description 37
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000460 chlorine Substances 0.000 claims abstract description 26
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 36
- VZIQXGLTRZLBEX-UHFFFAOYSA-N 2-chloro-1-propanol Chemical compound CC(Cl)CO VZIQXGLTRZLBEX-UHFFFAOYSA-N 0.000 claims description 26
- 239000012429 reaction media Substances 0.000 claims description 22
- 239000012071 phase Substances 0.000 claims description 15
- 230000009471 action Effects 0.000 claims description 14
- XENVCRGQTABGKY-ZHACJKMWSA-N chlorohydrin Chemical compound CC#CC#CC#CC#C\C=C\C(Cl)CO XENVCRGQTABGKY-ZHACJKMWSA-N 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000007921 spray Substances 0.000 claims description 8
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 7
- 239000013505 freshwater Substances 0.000 claims description 7
- 230000008676 import Effects 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- 238000004886 process control Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- 238000005660 chlorination reaction Methods 0.000 claims description 3
- 230000003020 moisturizing effect Effects 0.000 claims description 3
- 238000006396 nitration reaction Methods 0.000 claims description 3
- 239000012495 reaction gas Substances 0.000 claims description 3
- 235000019600 saltiness Nutrition 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 238000007127 saponification reaction Methods 0.000 claims description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000002912 waste gas Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000008878 coupling Effects 0.000 description 2
- 238000010168 coupling process Methods 0.000 description 2
- 238000005859 coupling reaction Methods 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- FGRBYDKOBBBPOI-UHFFFAOYSA-N 10,10-dioxo-2-[4-(N-phenylanilino)phenyl]thioxanthen-9-one Chemical compound O=C1c2ccccc2S(=O)(=O)c2ccc(cc12)-c1ccc(cc1)N(c1ccccc1)c1ccccc1 FGRBYDKOBBBPOI-UHFFFAOYSA-N 0.000 description 1
- TVEXGJYMHHTVKP-UHFFFAOYSA-N 6-oxabicyclo[3.2.1]oct-3-en-7-one Chemical compound C1C2C(=O)OC1C=CC2 TVEXGJYMHHTVKP-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- Epoxy Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A closed-circulation chlorohydrination reactor and its method during production of epoxypropane are disclosed. It consists of chlorine injector, propene jet pump, vapor-liquid separator, chlorohydrination tower, condenser on top of tower; one side of pre-reaction water pipe is connected with circulation pump, another side is connected with chlorine injector; one side of acid-mixing pipe is connected with chlorine injector, another side is connected with propene jet pump; one side of chlorprocohol reacting pipe is connected with propene jet pump, another side is connected with vapor-liquid separator entrance, lower outlet of vapor-liquid separator is connected with circulation pump entrance by water-feeding pipeline, which forms into circulation-piping reactive system, chlorine distributorand propene distributor are installed inside chlorohydrination tower; waste-gas exhaust pipe of condenser is connected with tailed gas circulation recovering apparatus entrance, condenser is connectedwith chlorohydrination tower by condensate liquor outputting pipe and propene feeding pipe is connected with tailed-gas circulation recovering apparatus by circulation recovering air pipe. It costs low, saves water usage, has more yield and no environmental pollution.
Description
Technical field
The present invention relates to the device and method that a kind of Chemicals are produced, what be specifically related to is closed cycle chlorohydrin action device and method in the propylene oxide production process.
Background technology
Critical process is the chlorohydrination operation in the propylene oxide by chlorohydrination production process, this operation is reaction medium with water, chlorine and water reaction generate hydrochloric acid and hypochlorous acid, hypochlorous acid generates propylene chlorohydrin with the propylene reaction that feeds again, wherein propylene chlorohydrin concentration mostly is 2.5～5.5% (wt), thereby the reaction water consumption is very big.The propylene chlorohydrin solution that generates carries out saponification reaction again and generates crude propene oxide after buffered.
In the former propylene oxide production process chlorohydrin action with fresh service water as reaction medium, this technical maturity, but water consumption quota is higher, power consumption is big, and because wastewater treatment capacity is big, has increased the weight of the environmental pollution degree.
Summary of the invention
Closed cycle chlorohydrin action device in the propylene oxide production process that the purpose of this invention is to provide a kind of production efficiency height, cost is low, the water consumption is little, alleviates environmental pollution.
Another object of the present invention provides chlorohydrin action method in a kind of propylene oxide production process.
The technical solution used in the present invention is:
Closed cycle chlorohydrin action device in the propylene oxide production process, comprise the chlorine injector, the propylene squirt pump, gas-liquid separator, the chlorohydrination tower, overhead condenser, tail gas loops back receiving apparatus, working shaft is equipped with water supply line, pass through the reaction water pipe coupling between working shaft and the recycle pump, pre-reaction water pipe one end is connected with recycle pump, the other end is connected with the chlorine injector, nitration mixture Guan Yiduan is connected with the chlorine injector, the other end is connected with the propylene injector, propylene chlorohydrin reaction tubes one end is connected with the propylene injector, the other end is connected with the gas-liquid separator inlet, the low outlet of gas-liquid separator is connected by the moisturizing pipeline with pump entry, constitute the circulation tubular reactor system thus, the high outlet of gas-liquid separator is passed through the gas-liquid mixed pipe coupling with chlorohydrination tower lower inlet, chlorine gas distributor and propylene sparger are installed in the chlorohydrination tower from bottom to top in proper order, reaction gas phase Guan Yiduan is connected with chlorohydrination tower upper outlet, the other end is connected with condenser inlet, the exhaust pipe of condenser loops back the receiving apparatus inlet with tail gas and links to each other, condenser is connected with the chlorohydrination tower by the phlegma output tube, the chlorohydrination tower is equipped with propylene chlorohydrin product output tube, the propylene sparger loops back receiving apparatus by the recovery circulating gas pipe with tail gas and is connected, and tail gas loops back receiving apparatus exhaust pipe is installed.
Chlorohydrin action method in the propylene oxide production process, technological process comprises: the reaction medium from saponifying process enters working shaft, be delivered to the propylene chlorohydrin pump entry, after boosting, the propylene chlorohydrin recycle pump in the circulation tubular reactor system, circulates, generate mixed acid solution (1.0～4.5) % (wt) with the chlorine reaction that sprays into through the import of chlorine injector gas phase, this mixed acid solution reacts with the propylene that propylene injector gas phase inlet sprays into again, generates propylene chlorohydrin solution (1.5～3.5) % (wt); Through gas-liquid separator separates, part gas-liquid mixture is at circulation tubular reactor system internal recycle, another part enters the continuation of chlorohydrination tower and chlorine, propylene react, improve propylene chlorohydrin concentration to (2.5～5.5) % (wt), liquid phase is the propylene chlorohydrin solution product, the gas phase gas that truncates loops back receiving apparatus and further handles, the recycled offgas of recovery with enter the chlorohydrination tower after raw material propylene mixes, tail gas is through the exhaust pipe emptying; Process control parameter comprises:
A, reaction can adopt the mixture of fresh water and lower concentration chlorination sodium water solution as reaction medium, also can adopt wherein a kind of as reaction medium, the reaction medium saltiness is between 0～6.5% (wt), and the reaction medium temperature is controlled at 20～70 ℃, and the reaction medium flow control is at 100M
3/ H～400M
3/ H;
B, propylene pressure-controlling are at 2～6Kgf/cm
2, chlorine gas pressure is controlled at 2～5Kgf/cm
2
C, reaction medium except that the mixture that can utilize fresh water and sodium chloride aqueous solution or one kind of, the fresh service water of also changeable use.
Advantage of the present invention is: greatly reduced the usage quantity of water, improved product yield, reduced the waste water control expense significantly and alleviated environmental pollution.
Description of drawings
Fig. 1 is the apparatus structure synoptic diagram of a kind of embodiment of the present invention.
Embodiment
Embodiment one
Closed cycle chlorohydrin action device in the propylene oxide production process, comprise chlorine injector 6, propylene squirt pump 8, gas-liquid separator 11, chlorohydrination tower 13, overhead condenser 15, tail gas loops back receiving apparatus 17, working shaft 2 is equipped with water supply line 1, be connected by reaction water pipe 3 between working shaft 2 and the recycle pump 4, pre-reaction water pipe 5 one ends are connected with recycle pump 4, the other end is connected with chlorine injector 6, nitration mixture pipe 7 one ends are connected with chlorine injector 6, the other end is connected with propylene injector 8, propylene chlorohydrin reaction tubes 9 one ends are connected with propylene injector 8, the other end is connected with gas-liquid separator 11 inlets, gas-liquid separator 11 low outlets are connected by moisturizing pipeline 10 with recycle pump 4 inlets, constitute the circulation tubular reactor system thus, gas-liquid separator 11 high outlets are connected by gas-liquid mixed pipe 12 with chlorohydrination tower 13 lower inlets, chlorine gas distributor 22 and propylene sparger 21 are installed in the chlorohydrination tower 13 from bottom to top in proper order, reaction gas phase pipe 14 1 ends are connected with chlorohydrination tower 13 upper outlets, the other end is connected with condenser 15 inlets, the exhaust pipe 16 and the tail gas of condenser 15 loops back receiving apparatus 17 inlets and links to each other, condenser 15 is connected with chlorohydrination tower 13 by phlegma output tube 19, chlorohydrination tower 13 is equipped with propylene chlorohydrin product output tube 20, propylene sparger 21 loops back receiving apparatus 17 by recovery circulating gas pipe 23 with tail gas and is connected, and tail gas loops back receiving apparatus 17 exhaust pipe 18 is installed.
Closed cycle chlorohydrin action method in the propylene oxide production process, technological process comprises: the fresh water from saponifying process enters working shaft 2 as reaction medium, be delivered to propylene chlorohydrin recycle pump 4 inlets, after boosting, propylene chlorohydrin recycle pump 4 in the circulation tubular reactor system, circulates, generate mixed acid solution 4% (wt) with the chlorine reaction that sprays into through the 6 gas phase imports of chlorine injector, this mixed acid solution reacts with the propylene that propylene injector 8 gas phases inlet sprays into again, generates propylene chlorohydrin solution 3% (wt); Separate a part of gas-liquid mixture at circulation tubular reactor system internal recycle through gas-liquid separator 11, another part enters 13 continuation of chlorohydrination tower and chlorine, propylene react, improve propylene chlorohydrin concentration to 5% (wt), liquid phase is the propylene chlorohydrin solution product, the gas phase gas that truncates loops back receiving apparatus 17, further handle and reclaim recycled offgas and enter chlorohydrination tower 13 after raw material propylene mixes, tail gas is through exhaust pipe 18 emptyings; Process control parameter comprises:
A, medium adopt fresh water, and the salt amount is 0.15% (wt);
B, reaction medium reaction mixture temperature are controlled at 40 ℃, and the reaction medium flow control is at 300M
3/ H;
C, propylene pressure-controlling are at 5Kgf/cm
2, chlorine gas pressure is controlled at 4Kgf/cm
2
Embodiment two
Embodiment two and embodiment one are basic identical, its difference is: generate mixed acid solution 3.5% (wt) with the chlorine reaction that sprays into through the 6 gas phase imports of chlorine injector, this mixed acid solution reacts with the propylene that propylene injector 8 gas phases inlet sprays into again, generates propylene chlorohydrin solution 2.5% (wt); Separate through gas-liquid separator 11, part gas-liquid mixture is at circulation tubular reactor system internal recycle, another part enters 13 continuation of chlorohydrination tower and chlorine, propylene react, improve propylene chlorohydrin concentration to 5% (wt), liquid phase is the propylene chlorohydrin solution product, the gas phase gas that truncates loops back receiving apparatus 17 and further handles back, receives recycled offgas and enters chlorohydrination tower 13 after raw material propylene mixes, and tail gas is through exhaust pipe 18 emptyings; Process control parameter comprises:
A, medium adopt the mixture of fresh water and lower concentration chlorination sodium water solution, and saltiness is 4% (wt);
B, reaction medium reaction mixture temperature are controlled at 50 ℃, and the reaction medium flow control is at 350M
3/ H;
C, propylene pressure-controlling are at 4.5Kgf/cm
2, chlorine gas pressure is controlled at 3.4Kgf/cm
2
Claims (4)
1, closed cycle chlorohydrin action device in the propylene oxide production process, comprise chlorine injector (6), propylene injector (8), gas-liquid separator (11), chlorohydrination tower (13), overhead condenser (15), tail gas loops back receiving apparatus (17), working shaft (2) is equipped with water supply line (1), be connected by reaction water pipe (3) between working shaft (2) and the recycle pump (4), it is characterized in that: pre-reaction water pipe (5) one ends are connected with recycle pump (4), the other end is connected with chlorine injector (6), nitration mixture pipe (7) one ends are connected with chlorine injector (6), the other end is connected with propylene injector (8), propylene chlorohydrin reaction tubes (9) one ends are connected with propylene injector (8), the other end is connected with gas-liquid separator (11) inlet, the low outlet of gas-liquid separator (11) is connected by moisturizing pipeline (10) with recycle pump (4) inlet, constitute the circulation tubular reactor system thus, the high outlet of gas-liquid separator (11) is connected by gas-liquid mixed pipe (12) with chlorohydrination tower (13) lower inlet, chlorine gas distributor (22) and propylene sparger (21) are installed in the chlorohydrination tower (13) from bottom to top in proper order, reaction gas phase pipe (14) one ends are connected with chlorohydrination tower (13) upper outlet, the other end is connected with overhead condenser (15) inlet, overhead condenser (15) exhaust pipe (16) loops back receiving apparatus (17) inlet with tail gas and links to each other, overhead condenser (15) is connected with chlorohydrination tower (13) by phlegma output tube (19), chlorohydrination tower (13) is equipped with propylene chlorohydrin product output tube (20), propylene sparger (21) loops back receiving apparatus (17) by recovery circulating gas pipe (23) with tail gas and is connected, and tail gas loops back receiving apparatus (17) exhaust pipe (18) is installed.
2, closed cycle chlorohydrin action method in the propylene oxide production process, technological process comprises: the reaction medium from saponifying process enters working shaft (2), be delivered to recycle pump (4) inlet, it is characterized in that: after recycle pump (4) boosts, in the circulation tubular reactor system, circulate, generate mixed acid solution 1.0～4.5% (wt) with the chlorine reaction that sprays into through chlorine injector (6) gas phase import, this mixed acid solution reacts with the propylene that propylene injector (8) gas phase inlet sprays into again, generates propylene chlorohydrin solution 1.5～3.5% (wt); Separate through gas-liquid separator (11), part gas-liquid mixture is at circulation tubular reactor system internal recycle, another part enters (13) continuation of chlorohydrination tower and chlorine, propylene react, improve propylene chlorohydrin concentration to 2.5～5.5% (wt), liquid phase is the propylene chlorohydrin solution product, the gas phase gas that truncates loops back receiving apparatus (17) and further handles, and reclaims recycled offgas and enters chlorohydrination tower (13) after raw material propylene mixes, and tail gas is through exhaust pipe (18) emptying;
Process control parameter comprises:
A, reaction adopt fresh water or lower concentration chlorination sodium water solution or the mixture of the two as reaction medium, and the reaction medium saltiness is between 0～6.5% (wt), and the reaction medium temperature is controlled at 20～70 ℃, and the reaction medium flow control is at 100M
3/ H～400M
3/ H;
B, propylene pressure-controlling are at 2～6Kgf/cm
2, chlorine gas pressure is controlled at 2～5Kgf/cm
2
3, closed cycle chlorohydrin action method in the propylene oxide production process according to claim 2 is characterized in that: the fresh service water of the also changeable use of reaction medium.
4, closed cycle chlorohydrin action method in the propylene oxide production process according to claim 2, it is characterized in that: reaction medium is closed cycle in whole technological process, be that propylene chlorohydrin solution carries out saponification behind the chlorohydrin action, through concentration, the fresh water part is returned the chlorohydrination operation as reaction medium afterwards.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710011074A CN100590121C (en) | 2007-04-23 | 2007-04-23 | Close-circulating chlorohydrination reactor and reactive method during production of epoxy-propane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710011074A CN100590121C (en) | 2007-04-23 | 2007-04-23 | Close-circulating chlorohydrination reactor and reactive method during production of epoxy-propane |
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| Publication Number | Publication Date |
|---|---|
| CN101074216A CN101074216A (en) | 2007-11-21 |
| CN100590121C true CN100590121C (en) | 2010-02-17 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399606B (en) * | 2015-12-18 | 2018-02-02 | 山东蓝星东大化工有限责任公司 | Technique for recovering propylene in expoxy propane subtractive process |
| CN111099964B (en) * | 2018-10-25 | 2022-10-21 | 中国石油化工股份有限公司 | Chlorohydrination reaction system and reaction method |
| CN111454179B (en) * | 2020-05-08 | 2023-10-20 | 河南金鹏化工有限公司 | Device and continuous process for producing methyl isocyanate from dimethyl sulfate |
| CN114249630A (en) * | 2020-09-24 | 2022-03-29 | 北京诺维新材科技有限公司 | Preparation method and application of chlorohydrin |
-
2007
- 2007-04-23 CN CN200710011074A patent/CN100590121C/en active Active
Non-Patent Citations (4)
| Title |
|---|
| 氯醇法制环氧丙烷的国外技术进展. 陈凯平.氯碱工业，第2期. 2000 |
| 氯醇法制环氧丙烷的国外技术进展. 陈凯平.氯碱工业，第2期. 2000 * |
| 氯醇法环氧丙烷生产装置的工艺优化及扩产改造. 李井辉等.氯碱工业，第5期. 2005 |
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| CN101074216A (en) | 2007-11-21 |
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