CN105498260A - High-efficiency and energy-saving caprolactam recovery technology - Google Patents
High-efficiency and energy-saving caprolactam recovery technology Download PDFInfo
- Publication number
- CN105498260A CN105498260A CN201510868690.7A CN201510868690A CN105498260A CN 105498260 A CN105498260 A CN 105498260A CN 201510868690 A CN201510868690 A CN 201510868690A CN 105498260 A CN105498260 A CN 105498260A
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- film evaporator
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- falling film
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/26—Multiple-effect evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D223/00—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom
- C07D223/02—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings
- C07D223/06—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D223/08—Oxygen atoms
- C07D223/10—Oxygen atoms attached in position 2
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/30—Improvements relating to adipic acid or caprolactam production
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention relates to an aqueous caprolactam solution concentration method. The method comprises steps as follows: 1), extract water is preheated through a heat exchanger by the aid of a pump I, and enters an evaporation pipe through a top inlet of a single-effect falling-film evaporator; 2), the extract water is distributed by an in-tower liquid distributor, is distributed in a heat exchange pipe in a film-like mode and is subjected to thin film evaporation through steam heating outside the pipe when entering a pipe cavity by the aid of gravity flow, and the extract water and secondary steam in the pipe flow down to the bottom of an effect body and enter a single-effect separation tank for liquid-steam separation; 3), a concentrated solution at the bottom of the effect body and the bottom of the separation tank is sent to the top of a two-effect falling-film evaporator through a pump II, and the concentrated solution of the two-effect falling-film evaporator is subjected to liquid-steam separation through a pump III, a pump IV and a two-effect separation tank; 4), the concentrated solution is sucked by a pump V from the bottom of the effect body and sent into the top of a three-effect falling-film evaporator for circulating concentration, and the technological requirement is met.
Description
Technical field
The present invention relates to a kind of energy-efficient caprolactam water solution concentration technology, adopt falling film evaporation and add the process route of thermal with function of mechanical steam recompression machine
Technical background
It is a balanced reaction that nylon 6/poly closes reaction, monomer caprolactam and the cyclic oligomer of about 8% ~ 10% is inevitably produced in production, these cyclic oligomers, particularly cyclic dimer, serious harm can be produced to polymerization process, adopt the deionized water of about 1:1 to carry out extracting and washing to nylon 6 slice after polymerization in actual production, the deionized water after extraction becomes the extraction water containing have an appointment 10% caprolactam and oligomer, need carry out concentration and recovery recycling.
Traditional caprolactam water concentration technology is generally triple effect evaporation technique, 1.0MPa (G) steam is needed directly to heat caprolactam water solution as thermal source in production process, the indirect steam that last effect evaporation and concentration produces has emitted usually because heat enthalpy value is low after water quench becomes, and the larger operating cost of energy consumption consumption is higher.Particularly current nylon 6/poly closes Large Copacity fast development, and recycling amount is also got up larger, if effectively reduce costs, is more conducive to the development of enterprise.
The present invention compresses from evaporimeter low-temperature level indirect steam out through compressor, makes it temperature, pressure improves, and heat content increases, and the heating clamber then sending back to evaporimeter is used as heating steam and is used, and heating steam itself is then condensed into water.Like this, the steam originally do not wanted just is fully utilized, and has fully reclaimed the latent heat of steam, has turn improved the thermal efficiency.The present invention makes full use of the latent heat of waste steam, and energy-efficient the concentrating of caprolactam water solution of nylon 6/poly being closed the low concentration produced in extraction workshop section carries out recycling.Not only greatly can reduce energy consumption, and evaporation equipment is compact, floor space is little, has effectively saved cost.
Summary of the invention
A kind of method containing the extraction water of caprolactam and its oligomer obtained after the invention provides concentrated production nylon 6 slice, described method, step is as follows:
1) extraction water is carried out being preheated to about 110 DEG C through heat exchanger (E-101) by pump (P-101), is entered in evaporation tube by effect falling film evaporator (E-102) top entry.
2) extraction water liquid distributor in the tower of (E-102) distributes, be distributed in heat exchanger tube with membranaceous, thin film evaporation is carried out by the Steam Heating outside pipe when entering tube chamber by means of gravity current, and run underneath in pipe together bottom effect body with indirect steam and enter an effect knockout drum (V-102) and carry out the separation of liquid vapour
3) to imitate bottom body and bottom knockout drum, concentration reaches 12% ~ 15% concentrate and sends into two effect falling film evaporator (E-103) tops with about 120 DEG C by pump (P-102), two effect falling film evaporator (E-103) concentrates carry out liquid vapour through pump (P-103, P-104) with two effects knockout drum (V-103) and are separated
4) concentrate is concentrated to about 45% and bottom effect body, sucks feeding triple effect falling film evaporator (E-104) top with ~ 120 DEG C by pump (P-105), carries out concentrated 70 ~ 75% concentrated concentration reaching technological requirement that circulate.
Process conditions of the present invention are as follows:
0.3MPa (G) raw steam equilibrium establishment is first used during driving.
After producing normal operation, concentrated material through two, the evaporation of triple effect falling film evaporator time, produce <0.1MPa (G), ~ indirect steam of 120 DEG C from two effect knockout drum tops enter first order compressor (C-101) carry out first time heat supercharging after enter high stage compressor (C-102) again, after secondary booster heats, indirect steam pressure improves 1.5 ~ 1.6 times, and temperature improves 1.05 ~ 1.1 times.The supercharged, secondary steam that heats accounting for total amount 90% is sent to an effect falling film evaporator (E-102), and all the other 10% are sent to the thermal source that triple effect falling film evaporator (E-104) needs as material concentration and evaporation.
One effect falling film evaporator (E-102) is by an isolated indirect steam in effect knockout drum (V-102) top, temperature is about 120 DEG C, pressure > 0.1MPa (G) enthalpy is higher, is directly sent to for material concentration and evaporation.After each flash-pot completes heat exchange, indirect steam becomes condensed water, is all collected in condensate water pot (V-101), is delivered to after heat exchanger (E-101) carries out preheating to starting material discharge by pump (P-107).
Calculate through reality, adopt traditional three-effect evaporation and condensation technique, concentrated 10 times of the low-concentration caprolactam water solution of unit per ton, need to consume about 0.3 ton of steam and 16.5 tons of cooling waters, operating cost about 72 yuan, this patent process route, need to consume about 16kW and 0.5 ton cooling water, operating cost about 13 yuan, cost reduces 80%, has good development potentiality.
Technology of the present invention and technological parameter are through screening acquisition, and see embodiment 1 through screening the preferred plan of the present invention obtained, compared to the prior art, unit ton product energy consumption index is as follows in the present invention:
From above index, the present invention is better than prior art.
This technique is adopted to have following characteristics:
Make full use of the latent heat of low-temperature level indirect steam, except start up, without the need to raw steam in whole evaporation process, greatly reduce raw steam consumption.
After heating steam source release heat is used as by the heating clamber delivering to evaporimeter of compressor compression heat content increase indirect steam, has condensed water of one's own, no longer needs water quench, save cooling water amount.
The main compressor electric consumption of operating cost, cost is lower.
Evaporation equipment is compact, and floor space is little, requisite space is also little.
Whole evaporation process is easy to operate,
Accompanying drawing illustrates:
Fig. 1 is apparatus and process flow chart.
Detailed description of the invention:
Further illustrate the present invention by the following examples.
Embodiment 1
The method containing the extraction water of caprolactam and its oligomer obtained after concentrated production nylon 6 slice, described method, step is as follows:
1) extraction water is carried out being preheated to about 110 DEG C through heat exchanger (E-101) by pump (P-101), is entered in evaporation tube by effect falling film evaporator (E-102) top entry.
2) extraction water liquid distributor in the tower of (E-102) distributes, be distributed in heat exchanger tube with membranaceous, thin film evaporation is carried out by the Steam Heating outside pipe when entering tube chamber by means of gravity current, and run underneath in pipe together bottom effect body with indirect steam and enter an effect knockout drum (V-102) and carry out the separation of liquid vapour
3) to imitate bottom body and bottom knockout drum, concentration reaches 12% ~ 15% concentrate and sends into two effect falling film evaporator (E-103) tops with about 120 DEG C by pump (P-102), two effect falling film evaporator (E-103) concentrates carry out liquid vapour through pump (P-103, P-104) with two effects knockout drum (V-103) and are separated
4) concentrate is concentrated to about 45% and bottom effect body, sucks feeding triple effect falling film evaporator (E-104) top with ~ 120 DEG C by pump (P-105), carries out concentrated 70 ~ 75% concentrated concentration reaching technological requirement that circulate.
Process conditions of the present invention are as follows:
0.3MPa (G) raw steam equilibrium establishment is first used during driving.
After producing normal operation, concentrated material through two, the evaporation of triple effect falling film evaporator time, produce <0.1MPa (G), ~ indirect steam of 120 DEG C from two effect knockout drum tops enter first order compressor (C-101) carry out first time heat supercharging after enter high stage compressor (C-102) again, after secondary booster heats, indirect steam pressure improves 1.5 ~ 1.6 times, and temperature improves 1.05 ~ 1.1 times.The supercharged, secondary steam that heats accounting for total amount 90% is sent to an effect falling film evaporator (E-102), and all the other 10% are sent to the thermal source that triple effect falling film evaporator (E-104) needs as material concentration and evaporation.
One effect falling film evaporator (E-102) is by an isolated indirect steam in effect knockout drum (V-102) top, temperature is about 120 DEG C, pressure > 0.1MPa (G) enthalpy is higher, is directly sent to for material concentration and evaporation.After each flash-pot completes heat exchange, indirect steam becomes condensed water, is all collected in condensate water pot (V-101), is delivered to after heat exchanger (E-101) carries out preheating to starting material discharge by pump (P-107).
Claims (2)
1. a caprolactam water solution method for concentration, described method step is as follows:
1) extraction water is carried out being preheated to about 110 DEG C through heat exchanger (E-101) by pump (P-101), enters in evaporation tube by effect falling film evaporator (E-102) top entry;
2) extraction water liquid distributor in the tower of (E-102) distributes, be distributed in heat exchanger tube with membranaceous, thin film evaporation is carried out by the Steam Heating outside pipe when entering tube chamber by means of gravity current, and run underneath in pipe together bottom effect body with indirect steam and enter an effect knockout drum (V-102) and carry out the separation of liquid vapour
3) to imitate bottom body and bottom knockout drum, concentration reaches 12% ~ 15% concentrate and sends into two effect falling film evaporator (E-103) tops with about 120 DEG C by pump (P-102), two effect falling film evaporator (E-103) concentrates carry out liquid vapour through pump (P-103, P-104) with two effects knockout drum (V-103) and are separated
4) concentrate is concentrated to about 45% and bottom effect body, sucks feeding triple effect falling film evaporator (E-104) top with ~ 120 DEG C by pump (P-105), carries out concentrated 70 ~ 75% concentrated concentration reaching technological requirement that circulate.
2. method according to claim 1, is characterized in that, wherein process conditions are as follows: first use 0.3MPa (G) raw steam equilibrium establishment during driving;
After producing normal operation, concentrated material is through two, during the evaporation of triple effect falling film evaporator, produce <0.1MPa (G), the indirect steam of ~ 120 DEG C from two effect knockout drum tops enter first order compressor (C-101) carry out first time heat supercharging after enter high stage compressor (C-102) again, after secondary booster heats, indirect steam pressure improves 1.5 ~ 1.6 times, temperature improves 1.05 ~ 1.1 times, the supercharged, secondary steam that heats accounting for total amount 90% is sent to an effect falling film evaporator (E-102), all the other 10% are sent to the thermal source that triple effect falling film evaporator (E-104) needs as material concentration and evaporation,
One effect falling film evaporator (E-102) is by an isolated indirect steam in effect knockout drum (V-102) top, temperature is about 120 DEG C, pressure > 0.1MPa (G) enthalpy is higher, directly be sent to for material concentration and evaporation, after each flash-pot completes heat exchange, indirect steam becomes condensed water, all be collected in condensate water pot (V-101), delivered to after heat exchanger (E-101) carries out preheating to starting material by pump (P-107) and discharge.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510868690.7A CN105498260A (en) | 2015-12-01 | 2015-12-01 | High-efficiency and energy-saving caprolactam recovery technology |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510868690.7A CN105498260A (en) | 2015-12-01 | 2015-12-01 | High-efficiency and energy-saving caprolactam recovery technology |
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| CN105498260A true CN105498260A (en) | 2016-04-20 |
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| CN201510868690.7A Pending CN105498260A (en) | 2015-12-01 | 2015-12-01 | High-efficiency and energy-saving caprolactam recovery technology |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858767A (en) * | 2016-06-16 | 2016-08-17 | 恒天中纤纺化无锡有限公司 | Nylon-6 chip monomer water recovery system |
| CN106007146A (en) * | 2016-06-30 | 2016-10-12 | 杭州聚合顺新材料股份有限公司 | Triple-effect evaporation condensate water re-purification method |
| CN106039749A (en) * | 2016-08-10 | 2016-10-26 | 中建安装工程有限公司 | Aqueous caprolactam solution concentration and reuse apparatus and technology thereof |
| CN106310689A (en) * | 2016-08-19 | 2017-01-11 | 江苏民生重工有限公司 | Energy-saving environment-friendly alkali evaporation system |
| CN106362426A (en) * | 2016-08-29 | 2017-02-01 | 常州中源工程技术有限公司 | Glycerin evaporation device and evaporation method thereof |
| CN106474755A (en) * | 2016-09-27 | 2017-03-08 | 深圳市瑞升华科技股份有限公司 | Integral type falling film evaporation separator |
| CN106540471A (en) * | 2016-10-28 | 2017-03-29 | 广西大学 | A kind of employing triple effect evaporation technique concentrates the method and device of biogas slurry |
| CN111013170A (en) * | 2019-12-26 | 2020-04-17 | 聊城鲁西聚酰胺新材料科技有限公司 | Caprolactam water solution energy-saving evaporation system and method |
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| CN102989185A (en) * | 2012-11-26 | 2013-03-27 | 中国化学赛鼎宁波工程有限公司 | Production system of dehydrated caprolactam and method thereof |
| CN103495285A (en) * | 2013-09-25 | 2014-01-08 | 福建锦江科技有限公司 | Monomer recovery device for polyamide slice extraction water |
| CN103830921A (en) * | 2013-12-03 | 2014-06-04 | 长乐恒申合纤科技有限公司 | System and technology for evaporation concentration of extraction water |
| CN203763870U (en) * | 2014-03-10 | 2014-08-13 | 浙江美邦实业集团有限公司 | Caprolactam concentrating device for production of chinlon 6 slice |
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2015
- 2015-12-01 CN CN201510868690.7A patent/CN105498260A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102989185A (en) * | 2012-11-26 | 2013-03-27 | 中国化学赛鼎宁波工程有限公司 | Production system of dehydrated caprolactam and method thereof |
| CN103495285A (en) * | 2013-09-25 | 2014-01-08 | 福建锦江科技有限公司 | Monomer recovery device for polyamide slice extraction water |
| CN103830921A (en) * | 2013-12-03 | 2014-06-04 | 长乐恒申合纤科技有限公司 | System and technology for evaporation concentration of extraction water |
| CN203763870U (en) * | 2014-03-10 | 2014-08-13 | 浙江美邦实业集团有限公司 | Caprolactam concentrating device for production of chinlon 6 slice |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105858767A (en) * | 2016-06-16 | 2016-08-17 | 恒天中纤纺化无锡有限公司 | Nylon-6 chip monomer water recovery system |
| CN106007146A (en) * | 2016-06-30 | 2016-10-12 | 杭州聚合顺新材料股份有限公司 | Triple-effect evaporation condensate water re-purification method |
| CN106039749A (en) * | 2016-08-10 | 2016-10-26 | 中建安装工程有限公司 | Aqueous caprolactam solution concentration and reuse apparatus and technology thereof |
| CN106310689A (en) * | 2016-08-19 | 2017-01-11 | 江苏民生重工有限公司 | Energy-saving environment-friendly alkali evaporation system |
| CN106362426A (en) * | 2016-08-29 | 2017-02-01 | 常州中源工程技术有限公司 | Glycerin evaporation device and evaporation method thereof |
| CN106362426B (en) * | 2016-08-29 | 2018-05-18 | 常州中源工程技术有限公司 | Glycerine vaporising device and its method of evaporating |
| CN106474755A (en) * | 2016-09-27 | 2017-03-08 | 深圳市瑞升华科技股份有限公司 | Integral type falling film evaporation separator |
| CN106474755B (en) * | 2016-09-27 | 2019-02-19 | 深圳市瑞升华科技股份有限公司 | Integral type falling film evaporation separator |
| CN106540471A (en) * | 2016-10-28 | 2017-03-29 | 广西大学 | A kind of employing triple effect evaporation technique concentrates the method and device of biogas slurry |
| CN106540471B (en) * | 2016-10-28 | 2019-02-19 | 广西大学 | A kind of method and device using triple effect evaporation technique concentration biogas slurry |
| CN111013170A (en) * | 2019-12-26 | 2020-04-17 | 聊城鲁西聚酰胺新材料科技有限公司 | Caprolactam water solution energy-saving evaporation system and method |
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