CN1454692A - Double-effect evaporating and crystallizing production process of low-solubility, easy-crystallizing and thermosensitive material - Google Patents

Double-effect evaporating and crystallizing production process of low-solubility, easy-crystallizing and thermosensitive material Download PDF

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Publication number
CN1454692A
CN1454692A CN 03137927 CN03137927A CN1454692A CN 1454692 A CN1454692 A CN 1454692A CN 03137927 CN03137927 CN 03137927 CN 03137927 A CN03137927 A CN 03137927A CN 1454692 A CN1454692 A CN 1454692A
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external circulation
circulation evaporator
effect
steam
evaporation crystallization
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CN 03137927
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CN1215895C (en
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史晓平
张继军
张英杰
王骞
郑献军
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GONGDA CHEMICAL EQUIPMENT CO Ltd SHIJIAZHUANG
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GONGDA CHEMICAL EQUIPMENT CO Ltd SHIJIAZHUANG
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Abstract

The invention is a double effect evaporation crystal craft for low solubility, easy to crystal, temperature-sensitive material. Parts of the second vapor distilled by the first effect appliance and the heated vapor which is put in continuously are pressed by the heat pump and are transmitted into the shell pass of the first appliance to be used as the heat source, the remanant second vapor distilled b the first effect appliance and the condensate discharged by the first outward circulation evaporator is put in the second outward circulation evaporator shell pass, the distilled vapor are used as the heat source of the second effect outward evaporator. Because that the water of the first effect appliance is used fully, it decreases the quantity of the vapor and the loss of heat energy.

Description

Low solubility, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology
Technical field
The present invention relates to a kind of low solubility, easily crystallization, heat sensitive material evaporative crystallization production technology, particularly a kind of improved low solubility, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology.
Background technology
In the prior art, low solubility, easily crystallization, heat sensitive material solution is subjected to its distinctive thermal sensitivity strong, concentration is low, the influence of characteristic factors such as easy crystallization, what evaporative crystallization production was adopted all is the single effect evaporation crystallizer, because the production process power consumption is high, it is big to steam water (steam) discharge capacity, steam water (steam) and condensed water exhaust temperature height, heat-energy losses is serious, the heat energy utilization rate is low, it is big with cooling water consumption that processing steams water, environmental protection control cost height, become the bottleneck that restriction is produced, evaporative crystallization production as L-Phenylglycine, L-Phenylglycine has another name called D acid, produce with biological fermentation process, main as amoxycillin, the raw material of semisynthetic antibiotics such as cynnematin, as a kind of important medicine intermediate, market prospects are very big, but present production process all is: produce D acid fermentation liquid with biological fermentation process earlier, adopt evaporation crystallization equipment that the water in the D acid fermentation liquid is evaporated again and make the D acid crystal, owing to be subjected to the distinctive temperature of D acid fermentation liquid can not be above 70 ℃, about concentration 2.5%, about solubility 3%, steaming the water yield reaches greatly and promptly occurs with mass crystallization in the evaporation process and influence that the resting period should not long characteristic factor, what its evaporative crystallization production was adopted mostly is by external circulation evaporator, vapour liquid separator, the single effect evaporation crystallizer that the clear liquid circulating pump constitutes, use the single effect evaporation crystallization production technology of such single effect evaporation crystallizer: 1 ton of D acid of every production all will steam 28 tons of water, will consume 1.1~1.5 tons of saturated vapors and whenever steam 1 ton of water, power consumption is high, in addition, the water that steams in a large number (steam) also is not utilized, except that a large amount of cooling water condensation of needs consumption, the water (steam) of discharging has also been taken away a large amount of heat energy, heat-energy losses is serious, is restricting the production of D acid.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes existing single effect evaporation crystallization production technology, and the thermal source that provides a kind of steam that goes out with the condensed water flash of the cover indirect steam that steams of evaporation crystallization equipment and discharge to make another set of evaporation crystallization equipment carries out low solubility, easily crystallization, the heat sensitive material evaporative crystallization production technology that evaporative crystallization is produced, promptly improved low solubility, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology.
The present invention solves the technical scheme that its technical problem takes: the thermal source that the steam that the condensed water flash of this indirect steam that steams with a cover evaporation crystallization equipment and discharge goes out is made another set of evaporation crystallization equipment carries out the low solubility that evaporative crystallization is produced, easily crystallization, heat sensitive material evaporative crystallization production technology, it is improved low solubility, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology, it adopts two cover evaporation crystallization equipments, one applies mechanically external circulation evaporator, vapour liquid separator, clear liquid circulating pump and heat pump are formed, do one and imitate evaporation crystallization equipment, one applies mechanically external circulation evaporator, vapour liquid separator and clear liquid circulating pump are formed, do two and imitate evaporation crystallization equipment, one imitates vapour liquid separator vaporization chamber boiling temperature is controlled at 55~65 ℃, two imitate vapour liquid separator vaporization chamber boiling temperature is controlled between 40~50 ℃, be to feed the thermal source that an effect external circulation evaporator shell side is made an effect external circulation evaporator after a part of and continuous heating steam that feeds of indirect steam that an effect evaporation crystallization equipment steams is pressurizeed by heat pump, the thermals source of the steam work two effect external circulation evaporators that the condensed water feeding two effect external circulation evaporator shell sides that an indirect steam that a remaining effect evaporation crystallization equipment steams and an effect external circulation evaporator are discharged flash off are produced, one imitate condensed water that external circulation evaporator discharges enter two imitate the external circulation evaporator shell sides flash off do two imitate the steam of external circulation evaporator thermals source after, mix flowing into the condensed water jar again with two condensed waters of imitating the external circulation evaporator discharge, the indirect steam that two effect evaporation crystallization equipments steam just enters condenser condenses.
Above-mentioned improved low solubility, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology, the condenser of employing can be a direct condenser; It also can be indirect condenser.
Above-mentioned improved low solubility, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology, an effect external circulation evaporator heating clamber temperature are controlled at 80~85 ℃, two effect external circulation evaporator heating clamber temperature are controlled between 55~60 ℃ is best.
This low solubility provided by the present invention, easily crystallization, heat sensitive material evaporative crystallization production technology is a kind of improved double-effect evaporation crystallization production technology, imitate indirect steam and that evaporation crystallization equipment steams with one and imitate the condensed water that external circulation evaporator discharges and make thermal source because two imitate evaporation crystallization equipments at the steam that two effect external circulation evaporator shell sides flash off, the water (steam) that one effect evaporation crystallization equipment is steamed is fully used, not only reduced the consumption of heating steam, but also reduced to steam the discharge capacity of water (steam), reduced the exhaust temperature that steams water (steam) and condensed water, reduced heat-energy losses, energy consumption is reduced, processing steams water and reduces with cooling water consumption, environmental protection control cost reduces, the heat energy utilization rate improves, and is more energy-conservation.
Description of drawings
Fig. 1 carries out the production equipment system schematic diagram that the L-Phenylglycine evaporative crystallization is produced for application improved low solubility provided by the present invention, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology.
The specific embodiment
Embodiment 1: embodiment 1 is an improved low solubility provided by the present invention, easily crystallization, the once application of heat sensitive material double-effect evaporation crystallization production technology in the L-Phenylglycine evaporative crystallization is produced, the embodiment of the invention 1 provides a kind of improved L-Phenylglycine double-effect evaporation crystallization production technology that the water yield is 5t/h of steaming, it adopts two cover evaporation crystallization equipments, one applies mechanically external circulation evaporator 11, vapour liquid separator 12, clear liquid circulating pump 13 and heat pump 14 are formed, do one and imitate evaporation crystallization equipment 1, one applies mechanically external circulation evaporator 21, vapour liquid separator 22 and clear liquid circulating pump 23 are formed, do two and imitate evaporation crystallization equipment 2, one imitates external circulation evaporator 11, two imitate external circulation evaporator 21 all adopts falling film evaporator, design:
One effect external circulation evaporator heating clamber temperature is 80 ± 5 ℃, vapour liquid separator vaporization chamber
Boiling temperature is 60 ± 5 ℃
Two effect external circulation evaporator heating clamber temperature are 60 ± 5 ℃, vapour liquid separator vaporization chamber
Boiling temperature is 45 ± 5 ℃
Original liquid concentration: 2.5%, temperature: 60~70 ℃, inlet amount: 6m 3/ h
Heating steam pressure: 0.6Mpa
Evaporating temperature :≤60 ℃
Finish concentration: 30%
Condensate temperature :≤32 ℃
With reference to accompanying drawing, this improved L-Phenylglycine double-effect evaporation crystallization production technology that the embodiment of the invention 1 is provided: will contain the D acid fermentation liquid 8 of 60~70 ℃ of D acid 2.5%, temperature with 6m by raw liquor pump 4 3The flow of/h is got in the external circulation evaporator of one, two effect evaporation crystallization equipments, and wherein an inlet amount of imitating external circulation evaporator 11 is 3.8m 3/ h, two inlet amounies of imitating external circulation evaporator 21 are 2.2m 3/ h, the zymotic fluid that enters an effect external circulation evaporator 11 enters an effect vapour liquid separator 12 and carries out vapor-liquid separation after heating, steaming temperature with the flow of 3.1t/h is 60 ± 5 ℃ indirect steam, after the high temperature foam removal, the flow of 1.2t/h and feed the shell side of an effect external circulation evaporator 11 with the heating steam 7 that the flow of 2t/h feeds continuously through heat pump 14 pressurization backs wherein, make the thermal source of an effect external circulation evaporator 11, remaining indirect steam feeds the shell side of two effect external circulation evaporators 21 with the flow of 1.9t/h; The temperature that one effect external circulation evaporator 11 is discharged with the flow of 3.2t/h is 80 ± 5 ℃ condensed water enters two effect external circulation evaporators 21 by U type pipe 3 a shell side, the steam that flashes off with the flow of 120kg/h and feed two with the flow of 1.9t/h and imitate one of external circulation evaporator shell sides and imitate indirect steam that evaporation crystallization equipments steam and make two thermals source of imitating external circulation evaporators 21, steam temperature and be 45 ± 5 ℃ indirect steam, after the high temperature foam removal, enter direct condenser 6 condensations.One imitates evaporation crystallization equipment 1 steams after temperature is 60 ± 5 ℃ indirect steam with the flow of 3.1t/h, remaining liquid is through eliminating supersaturation, clear liquid is got on the liquid distribution trough on an effect external circulation evaporator 11 tops again with an effect clear liquid circulating pump 13, mix with the stoste of continuous feeding and to be membranaceous by the tubulation inwall and to flow down, reheat; Two imitate evaporation crystallization equipments 2, and to steam temperature be behind 45 ± 5 ℃ the indirect steam, remaining liquid is through eliminating supersaturation, clear liquid is got on the liquid distribution trough on two effect external circulation evaporators, 21 tops again with two effect clear liquid circulating pumps 23, mix with the stoste of continuous feeding and to be membranaceous by the tubulation inwall and to flow down, reheat.One imitates and the D acid crystal of two effect vapour liquid separator bottom deposits, is discharged to centrifuge with discharging pump and carries out Separation of Solid and Liquid and get final product.One condensed water of imitating external circulation evaporator 11 discharges enters and mixes inflow condensed water jar 5 with two condensed waters of imitating external circulation evaporator 21 discharges after two effect external circulation evaporators, 21 shell sides flash off the steam of making two effect external circulation evaporator thermals source, and the flow of condensed water is 5.1t/h; The indirect steam that two effect evaporation crystallization equipments 2 steam just enters direct condenser 6 condensations, and the consumption of cooling water 9 is 55m 3/ h.
The L-Phenylglycine evaporative crystallization production technology that this steaming water yield that the embodiment of the invention 1 is provided is 5t/h, more traditional steaming water yield are the L-Phenylglycine single effect evaporation crystallization production technology of the 5t/h heating steam consumption that is not less than 5.5t/h, are not less than 140m 3The cooling water consumption of/h is saved heating steam 3.5t/h, cooling water 85m 3/ h.
Embodiment 2: embodiment 2 is improved low solubilities provided by the present invention, easily crystallization, another time application of heat sensitive material double-effect evaporation crystallization production technology in the L-Phenylglycine evaporative crystallization is produced, the embodiment of the invention 2 provides a kind of improved L-Phenylglycine double-effect evaporation crystallization production technology that the water yield is 10t/h of steaming, it adopts two cover evaporation crystallization equipments, one applies mechanically external circulation evaporator 11, vapour liquid separator 12, clear liquid circulating pump 13 and heat pump 14 are formed, do one and imitate evaporation crystallization equipment 1, one applies mechanically external circulation evaporator 21, vapour liquid separator 22 and clear liquid circulating pump 23 are formed, do two and imitate evaporation crystallization equipment 2, one imitates external circulation evaporator 11, two imitate external circulation evaporator 21 all adopts falling film evaporator, design:
One effect external circulation evaporator heating clamber temperature is 80 ± 5 ℃, vapour liquid separator vaporization chamber
Boiling temperature is 60 ± 5 ℃
Two effect external circulation evaporator heating clamber temperature are 60 ± 5 ℃, vapour liquid separator vaporization chamber
Boiling temperature is 45 ± 5 ℃
Original liquid concentration: 2.5%, temperature: 〉=40 ℃, inlet amount: 12m 3/ h
Heating steam pressure: 0.4Mpa
Evaporating temperature :≤60 ℃
Finish concentration: 30%
Condensate temperature :≤32 ℃
With reference to accompanying drawing, this improved L-Phenylglycine double-effect evaporation crystallization production technology that the embodiment of the invention 2 is provided: will contain the D acid fermentation liquid 8 of D acid 2.5%, temperature 〉=40 ℃ with 12m by raw liquor pump 4 3The flow of/h is got in the external circulation evaporator of one, two effect evaporation crystallization equipments, and wherein an inlet amount of imitating external circulation evaporator 11 is 7m 3/ h, two inlet amounies of imitating external circulation evaporator 21 are 5m 3/ h, the zymotic fluid that enters an effect external circulation evaporator 11 enters an effect vapour liquid separator 12 and carries out vapor-liquid separation after heating, steaming temperature with the flow of 6t/h is 60 ± 5 ℃ indirect steam, after the high temperature foam removal, the flow of 2t/h and feed the shell side of an effect external circulation evaporator 11 with the heating steam 7 that the flow of 4.4t/h feeds continuously through heat pump 14 pressurization backs wherein, make the thermal source of an effect external circulation evaporator 11, remaining indirect steam feeds the shell side of two effect external circulation evaporators 21 with the flow of 4t/h; The temperature that one effect external circulation evaporator 11 is discharged with the flow of 6.4t/h is 80 ± 5 ℃ condensed water enters two effect external circulation evaporators 21 by U type pipe 3 a shell side, the steam that flashes off with the flow of 250kg/h and feed two with the flow of 4t/h and imitate one of external circulation evaporator shell sides and imitate indirect steam that evaporation crystallization equipments steam and make two thermals source of imitating external circulation evaporators 21, steam temperature and be 45 ± 5 ℃ indirect steam, after the high temperature foam removal, enter indirect condenser 6 condensations.One imitates evaporation crystallization equipment 1 steams after temperature is 60 ± 5 ℃ indirect steam with the flow of 6t/h, remaining liquid is through eliminating supersaturation, clear liquid is got on the liquid distribution trough on an effect external circulation evaporator 11 tops again with an effect clear liquid circulating pump 13, mix with the stoste of continuous feeding and to be membranaceous by the tubulation inwall and to flow down, reheat; Two imitate evaporation crystallization equipments 2, and to steam temperature be behind 45 ± 5 ℃ the indirect steam, remaining liquid is through eliminating supersaturation, clear liquid is got on the liquid distribution trough on two effect external circulation evaporators, 21 tops again with two effect clear liquid circulating pumps 23, mix with the stoste of continuous feeding and to be membranaceous by the tubulation inwall and to flow down, reheat.One imitates and the D acid crystal of two effect vapour liquid separator bottom deposits, is discharged to centrifuge with discharging pump and carries out Separation of Solid and Liquid and get final product.One condensed water of imitating external circulation evaporator 11 discharges enters and mixes inflow condensed water jar 5 with two condensed waters of imitating external circulation evaporator 21 discharges after two effect external circulation evaporators, 21 shell sides flash off the steam of making two effect external circulation evaporator thermals source, and the flow of condensed water is 10.4t/h; The indirect steam that two effect evaporation crystallization equipments 2 steam just enters indirect condenser 6 condensations, and the consumption of cooling water 9 is 120m 3/ h.
The L-Phenylglycine evaporative crystallization production technology that this steaming water yield that the embodiment of the invention 2 is provided is 10t/h, more traditional steaming water yield are the L-Phenylglycine single effect evaporation crystallization production technology of the 10t/h heating steam consumption that is not less than 11t/h, are not less than 280m 3The cooling water consumption of/h is saved heating steam 6.6t/h, cooling water 160m 3/ h.

Claims (4)

1, a kind of low solubility, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology, it is characterized in that: it adopts two cover evaporation crystallization equipments, one applies mechanically external circulation evaporator (11), vapour liquid separator (12), clear liquid circulating pump (13) and heat pump (14) are formed, do one and imitate evaporation crystallization equipment (1), one applies mechanically external circulation evaporator (21), vapour liquid separator (22) and clear liquid circulating pump (23) are formed, do two and imitate evaporation crystallization equipment (2), one imitates vapour liquid separator vaporization chamber boiling temperature is controlled at 55~65 ℃, two imitate vapour liquid separator vaporization chamber boiling temperature is controlled between 40~50 ℃, be the indirect steam part that an effect evaporation crystallization equipment (1) steams to be passed through heat pump (14) pressurization back with the heating steam of feeding continuously feed the thermal source that an effect external circulation evaporator shell side work one is imitated external circulation evaporator (11), the thermals source of the steam work two effect external circulation evaporators (21) that the condensed water feeding two effect external circulation evaporator shell sides that an indirect steam that a remaining effect evaporation crystallization equipment (1) steams and an effect external circulation evaporator (11) are discharged flash off are produced, one imitate condensed water that external circulation evaporator (11) discharges enter two imitate the external circulation evaporator shell sides flash off do two imitate the steam of external circulation evaporator thermals source after, mix flowing into condensed water jar (5) again with two condensed waters of imitating external circulation evaporator (21) discharge, the indirect steam that two effect evaporation crystallization equipments (2) steam just enters condenser (6) condensation.
2, low solubility according to claim 1, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology is characterized in that: one imitates external circulation evaporator (11) heating clamber temperature is controlled at 80~85 ℃, two and imitates external circulation evaporator (21) heating clamber temperature and be controlled between 55~60 ℃.
3, low solubility according to claim 1, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology, it is characterized in that: one to imitate external circulation evaporator (11) heating clamber temperature be that 80 ± 5 ℃, vapour liquid separator (12) vaporization chamber boiling temperature are 60 ± 5 ℃, and two to imitate external circulation evaporator (21) heating clamber temperature be that 60 ± 5 ℃, vapour liquid separator (22) vaporization chamber boiling temperature are 45 ± 5 ℃.
4, according to claim 1,2 or 3 described low solubilities, easily crystallization, heat sensitive material double-effect evaporation crystallization production technology, it is characterized in that: an effect external circulation evaporator (11), two is imitated external circulation evaporators (21) and is all adopted falling film evaporator.
CN 03137927 2003-05-30 2003-05-30 Double-effect evaporating and crystallizing production process of low-solubility, easy-crystallizing and thermosensitive material Expired - Fee Related CN1215895C (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102807521A (en) * 2011-05-30 2012-12-05 江苏乐科热力科技有限公司 Concentrating crystallization process for tryptophan or glyphosate by using mechanical vapor recompression technology
CN102921185A (en) * 2012-10-31 2013-02-13 江阴丰力生化工程装备有限公司 Double-effect continuous crystallization device
CN103553255A (en) * 2013-10-31 2014-02-05 山东科信生物化学有限公司 Method for treating and utilizing wastewater in synthesis of tebufenozide insecticide
CN103657120A (en) * 2012-09-21 2014-03-26 中川工程顾问(上海)有限公司 Ultra-efficient energy-saving type vacuum concentration device and method
CN104307195A (en) * 2014-10-10 2015-01-28 上海远跃制药机械有限公司 Double-effect falling film MVR evaporation system

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102807521A (en) * 2011-05-30 2012-12-05 江苏乐科热力科技有限公司 Concentrating crystallization process for tryptophan or glyphosate by using mechanical vapor recompression technology
CN102807521B (en) * 2011-05-30 2015-01-28 江苏乐科热力科技有限公司 Concentrating crystallization process for tryptophan or glyphosate by using mechanical vapor recompression technology
CN103657120A (en) * 2012-09-21 2014-03-26 中川工程顾问(上海)有限公司 Ultra-efficient energy-saving type vacuum concentration device and method
CN103657120B (en) * 2012-09-21 2015-11-18 中川工程顾问(上海)有限公司 Ultra high efficiency energy-saving type vacuum enrichment facility and method
CN102921185A (en) * 2012-10-31 2013-02-13 江阴丰力生化工程装备有限公司 Double-effect continuous crystallization device
CN102921185B (en) * 2012-10-31 2015-04-22 江阴丰力生化工程装备有限公司 Double-effect continuous crystallization device
CN103553255A (en) * 2013-10-31 2014-02-05 山东科信生物化学有限公司 Method for treating and utilizing wastewater in synthesis of tebufenozide insecticide
CN103553255B (en) * 2013-10-31 2014-12-10 山东科信生物化学有限公司 Method for treating and utilizing wastewater in synthesis of tebufenozide insecticide
CN104307195A (en) * 2014-10-10 2015-01-28 上海远跃制药机械有限公司 Double-effect falling film MVR evaporation system
CN104307195B (en) * 2014-10-10 2016-04-13 上海远跃制药机械有限公司 Economic benefits and social benefits falling liquid film MVR vapo(u)rization system

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