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CN104892437A - Production technology for L-lysine hydrochloride - Google Patents

Production technology for L-lysine hydrochloride Download PDF

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Publication number
CN104892437A
CN104892437A CN201510247562.0A CN201510247562A CN104892437A CN 104892437 A CN104892437 A CN 104892437A CN 201510247562 A CN201510247562 A CN 201510247562A CN 104892437 A CN104892437 A CN 104892437A
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China
Prior art keywords
mother liquor
whizzer
filter
crystallizer
kilograms
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Pending
Application number
CN201510247562.0A
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Chinese (zh)
Inventor
曹嵘
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rong Tai Bio Tech Ltd Nantong
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Rong Tai Bio Tech Ltd Nantong
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Priority to CN201510247562.0A priority Critical patent/CN104892437A/en
Publication of CN104892437A publication Critical patent/CN104892437A/en
Pending legal-status Critical Current

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Abstract

The invention discloses a production technology for L-lysine hydrochloride. The technology includes the steps of: dissolution, filtration, centrifugation, washing, drying, inspection, and mother liquor recovery. The technology provided by the invention has the characteristics of easily available raw materials, low production cost, simple process, mild reaction conditions, yield up to 99%, and recyclable mother liquor. The process has the advantages of mild reaction, no waste gas or waste water, no danger, accordance with the current environmental protection and safety requirements, green production and safe production. And the L-lysine hydrochloride belongs to the state encouraged biological pharmaceutical products.

Description

A kind of production technique of LYS
Technical field
The invention belongs to medical applications field, be specifically related to a kind of production technique of LYS.
Background technology
LYS (40%, 35 DEG C) soluble in water, the aqueous solution is neutral to subacidity.Stable when relative humidity less than 60%, more than 60% then generates dihydrate.If lack Methionin in body, cause protein metabolism disturbance and dysfunction, cause retardation of growth.Due to the easy moisture absorption of Methionin, be often made into hydrochloride, 1g 1B is equivalent to 1.25gL-lysine hydrochloride.Usually more stable, easily lump under high humidity, slightly painted.This product is white crystals or crystalline powder; Odorless.Childhood development phase, ill rear decubation and pregnant lactication phase, higher to the nutritional requirement of Methionin.Alkaline condition and directly and reducing sugar there is lower heating and then decompose.263-264 DEG C melt and decompose.Bitter sweet.
Summary of the invention
Goal of the invention: the production technique that the invention provides a kind of LYS, the low technique of production cost is simple, and reaction conditions is gentle, and productive rate reaches 99%, and mother liquor can also recycled for multiple times.
Technical scheme: a kind of production technique of LYS, comprises the steps:
(1) dissolve: the pure water being put into 1400L in 1500L dissolving vessel by water pipe, start agitator to stir, then, drop into the lysine hydrochloride crude product of 500 kilograms, be warming up to 70 DEG C-75 DEG C dissolve after, add the gac of 50 kilograms, under the condition of 90 DEG C-95 DEG C, be incubated 15-20 minute;
(2) filter: complete filter paper, filter bag in the filter, open crystallizer vacuum, filtration under diminished pressure by filtrate suction filtration in crystallizer;
(3) centrifugal, washing: start crystallizer and stir, in cooling water temperature to tank 8 DEG C-10 DEG C, whizzer rejection filter 1 hour, with 10 kilogram of 95% washing with alcohol, crystal dries, and mother liquor is withdrawn in dissolving vessel, treats down to criticize and continues the use that feeds intake;
(4) it is dry: after crystallization is gone out whizzer, load in moisture eliminator, vacuum tightness state is dry, vacuum tightness must not higher than-0.06MPa, and after wet product enters moisture eliminator, temperature rises to 90 DEG C of needs 2.5-3 hour, if caking, re-start drying after pulverizing, temperature at 90-100 DEG C of successive drying, discharging in 2.5-3 hour;
(5) check: after dried material packages, carry out intermediate controlled chemical examination, after qualified, can carry out batch mixing, the method for batch mixing is every four to five dry batches, and to mix be a part; Then apply for checking and examination, qualified rear labeling, warehouse-in;
(6) disposing mother liquor: the concrete removal process of mother liquor is as follows:
After a, mother liquid recycle 10 batches, concentrating under reduced pressure in suction concentration tank;
B, when being concentrated into 1/2 volume, material is got rid of in cooling, and mother liquor is drawn back in concentration tank, and continue concentrated, cooling, gets rid of material; C, crystallization are as crude product.
As optimization: in described step (1), put into the pure water of 1400L by water pipe in 1500L dissolving vessel, start agitator to stir, then, drop into the lysine hydrochloride crude product of 500 kilograms, be warming up to 73 DEG C dissolve after, add the gac of 50 kilograms, under the condition of 92 DEG C be incubated 18 minutes.
As optimization: in described step (3), start crystallizer and stir, in cooling water temperature to tank 9 DEG C, whizzer rejection filter 1 hour, with 10 kilogram of 95% washing with alcohol, crystal dries, and mother liquor is withdrawn in dissolving vessel, treats down to criticize and continues the use that feeds intake.
As optimization: in described step (4), after crystallization is gone out whizzer, load in moisture eliminator, vacuum tightness state is dry, and vacuum tightness must not higher than-0.06MPa, after wet product enters moisture eliminator, temperature rises to 90 DEG C of needs 2.8 hours, if caking, re-starts drying after pulverizing, temperature at 94 DEG C of successive dryings, discharging in 2.7 hours.
As optimization: described centrifugal concrete operations: complete cloth bag, start whizzer, per minute 1200 turns, the time is 60 minutes.
Beneficial effect: raw material of the present invention is easy to get, the low technique of production cost is simple, reaction conditions is gentle, and productive rate reaches 99%, and mother liquor can also recycled for multiple times, this technological process reaction temperature and, without waste gas, waste water, without dangerous, adapt to the requirement of current Environmental Safety, green production, safety in production, belong to country and encourage class biological medicine product.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
Specific embodiment one:
A production technique for LYS, comprises the steps:
(1) dissolve: the pure water being put into 1400L in 1500L dissolving vessel by water pipe, start agitator and stir, then, drop into the lysine hydrochloride crude product of 500 kilograms, be warming up to 70 DEG C dissolve after, add the gac of 50 kilograms, under the condition of 90 DEG C be incubated 15 minutes;
(2) filter: complete filter paper, filter bag in the filter, open crystallizer vacuum, filtration under diminished pressure by filtrate suction filtration in crystallizer;
(3) centrifugal, washing: start crystallizer and stir, in cooling water temperature to tank 8 DEG C, whizzer rejection filter 1 hour, with 10 kilogram of 95% washing with alcohol, crystal dries, and mother liquor is withdrawn in dissolving vessel, treats down to criticize and continues the use that feeds intake;
(4) it is dry: after crystallization is gone out whizzer, load in moisture eliminator, vacuum tightness state is dry, vacuum tightness must not higher than-0.06MPa, and after wet product enters moisture eliminator, temperature rises to 90 DEG C of needs 2.5 hours, if caking, re-start drying after pulverizing, temperature at 90-100 DEG C of successive drying, discharging in 2.5 hours;
(5) check: after dried material packages, carry out intermediate controlled chemical examination, after qualified, can carry out batch mixing, the method for batch mixing is every four to five dry batches, and to mix be a part; Then apply for checking and examination, qualified rear labeling, warehouse-in;
(6) disposing mother liquor: the concrete removal process of mother liquor is as follows:
After a, mother liquid recycle 10 batches, concentrating under reduced pressure in suction concentration tank;
B, when being concentrated into 1/2 volume, material is got rid of in cooling, and mother liquor is drawn back in concentration tank, and continue concentrated, cooling, gets rid of material; C, crystallization are as crude product.
Described centrifugal concrete operations: complete cloth bag, start whizzer, per minute 1200 turns, the time is 60 minutes.
Specific embodiment two:
A production technique for LYS, comprises the steps:
(1) dissolve: the pure water being put into 1400L in 1500L dissolving vessel by water pipe, start agitator and stir, then, drop into the lysine hydrochloride crude product of 500 kilograms, be warming up to 75 DEG C dissolve after, add the gac of 50 kilograms, under the condition of 95 DEG C be incubated 20 minutes;
(2) filter: complete filter paper, filter bag in the filter, open crystallizer vacuum, filtration under diminished pressure by filtrate suction filtration in crystallizer;
(3) centrifugal, washing: start crystallizer and stir, in cooling water temperature to tank 10 DEG C, whizzer rejection filter 1 hour, with 10 kilogram of 95% washing with alcohol, crystal dries, and mother liquor is withdrawn in dissolving vessel, treats down to criticize and continues the use that feeds intake;
(4) dry: after crystallization is gone out whizzer, load in moisture eliminator, vacuum tightness state is dry, and vacuum tightness must not higher than-0.06MPa, after wet product enters moisture eliminator, temperature rises to 90 DEG C of needs 3 hours, if caking, re-start drying after pulverizing, temperature at 100 DEG C of successive dryings, discharging in 3 hours;
(5) check: after dried material packages, carry out intermediate controlled chemical examination, after qualified, can carry out batch mixing, the method for batch mixing is every four to five dry batches, and to mix be a part; Then apply for checking and examination, qualified rear labeling, warehouse-in;
(6) disposing mother liquor: the concrete removal process of mother liquor is as follows:
After a, mother liquid recycle 10 batches, concentrating under reduced pressure in suction concentration tank;
B, when being concentrated into 1/2 volume, material is got rid of in cooling, and mother liquor is drawn back in concentration tank, and continue concentrated, cooling, gets rid of material; C, crystallization are as crude product.
Described centrifugal concrete operations: complete cloth bag, start whizzer, per minute 1200 turns, the time is 60 minutes.
Specific embodiment three:
A production technique for LYS, comprises the steps:
(1) dissolve: the pure water being put into 1400L in 1500L dissolving vessel by water pipe, start agitator and stir, then, drop into the lysine hydrochloride crude product of 500 kilograms, be warming up to 73 DEG C dissolve after, add the gac of 50 kilograms, under the condition of 92 DEG C be incubated 18 minutes;
(2) filter: complete filter paper, filter bag in the filter, open crystallizer vacuum, filtration under diminished pressure by filtrate suction filtration in crystallizer;
(3) centrifugal, washing: start crystallizer and stir, in cooling water temperature to tank 9 DEG C, whizzer rejection filter 1 hour, with 10 kilogram of 95% washing with alcohol, crystal dries, and mother liquor is withdrawn in dissolving vessel, treats down to criticize and continues the use that feeds intake;
(4) it is dry: after crystallization is gone out whizzer, load in moisture eliminator, vacuum tightness state is dry, vacuum tightness must not higher than-0.06MPa, and after wet product enters moisture eliminator, temperature rises to 90 DEG C of needs 2.8 hours, if caking, re-start drying after pulverizing, temperature at 94 DEG C of successive dryings, discharging in 2.7 hours;
(5) check: after dried material packages, carry out intermediate controlled chemical examination, after qualified, can carry out batch mixing, the method for batch mixing is every four to five dry batches, and to mix be a part; Then apply for checking and examination, qualified rear labeling, warehouse-in;
(6) disposing mother liquor: the concrete removal process of mother liquor is as follows:
After a, mother liquid recycle 10 batches, concentrating under reduced pressure in suction concentration tank;
B, when being concentrated into 1/2 volume, material is got rid of in cooling, and mother liquor is drawn back in concentration tank, and continue concentrated, cooling, gets rid of material; C, crystallization are as crude product.
Described centrifugal concrete operations: complete cloth bag, start whizzer, per minute 1200 turns, the time is 60 minutes.
The present invention is not limited to above-mentioned preferred forms; anyone can draw other various forms of products under enlightenment of the present invention; no matter but any change is done in its shape or structure; every have identical with the application or akin technical scheme, all drops within protection scope of the present invention.

Claims (5)

1. a production technique for LYS, is characterized in that: comprise the steps:
(1) dissolve: the pure water being put into 1400L in 1500L dissolving vessel by water pipe, start agitator to stir, then, drop into the lysine hydrochloride crude product of 500 kilograms, be warming up to 70 DEG C-75 DEG C dissolve after, add the gac of 50 kilograms, under the condition of 90 DEG C-95 DEG C, be incubated 15-20 minute;
(2) filter: complete filter paper, filter bag in the filter, open crystallizer vacuum, filtration under diminished pressure by filtrate suction filtration in crystallizer;
(3) centrifugal, washing: start crystallizer and stir, in cooling water temperature to tank 8 DEG C-10 DEG C, whizzer rejection filter 1 hour, with 10 kilogram of 95% washing with alcohol, crystal dries, and mother liquor is withdrawn in dissolving vessel, treats down to criticize and continues the use that feeds intake;
(4) it is dry: after crystallization is gone out whizzer, load in moisture eliminator, vacuum tightness state is dry, vacuum tightness must not higher than-0.06MPa, and after wet product enters moisture eliminator, temperature rises to 90 DEG C of needs 2.5-3 hour, if caking, re-start drying after pulverizing, temperature at 90-100 DEG C of successive drying, discharging in 2.5-3 hour;
(5) check: after dried material packages, carry out intermediate controlled chemical examination, after qualified, can carry out batch mixing, the method for batch mixing is every four to five dry batches, and to mix be a part; Then apply for checking and examination, qualified rear labeling, warehouse-in;
(6) disposing mother liquor: the concrete removal process of mother liquor is as follows:
After a, mother liquid recycle 10 batches, concentrating under reduced pressure in suction concentration tank;
B, when being concentrated into 1/2 volume, material is got rid of in cooling, and mother liquor is drawn back in concentration tank, and continue concentrated, cooling, gets rid of material; C, crystallization are as crude product.
2. the production technique of LYS according to claim 1, it is characterized in that: in described step (1), put into the pure water of 1400L by water pipe in 1500L dissolving vessel, start agitator to stir, then, drop into the lysine hydrochloride crude product of 500 kilograms, be warming up to 73 DEG C dissolve after, add the gac of 50 kilograms, under the condition of 92 DEG C, be incubated 18 minutes.
3. the production technique of LYS according to claim 1, it is characterized in that: in described step (3), start crystallizer to stir, in cooling water temperature to tank 9 DEG C, whizzer rejection filter 1 hour, by 10 kilogram of 95% washing with alcohol, crystal dries, mother liquor is withdrawn in dissolving vessel, treats down to criticize and continues the use that feeds intake.
4. the production technique of LYS according to claim 1, it is characterized in that: in described step (4), after crystallization is gone out whizzer, load in moisture eliminator, vacuum tightness state is dry, vacuum tightness must not higher than-0.06MPa, and after wet product enters moisture eliminator, temperature rises to 90 DEG C of needs 2.8 hours, if caking, re-start drying after pulverizing, temperature at 94 DEG C of successive dryings, discharging in 2.7 hours.
5. the production technique of LYS according to claim 1, is characterized in that: described centrifugal concrete operations: complete cloth bag, and start whizzer, per minute 1200 turns, the time is 60 minutes.
CN201510247562.0A 2015-05-15 2015-05-15 Production technology for L-lysine hydrochloride Pending CN104892437A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105503630A (en) * 2015-12-04 2016-04-20 安徽丰原发酵技术工程研究有限公司 Method for purifying lysine hydrochloride
CN107501137A (en) * 2017-08-29 2017-12-22 东明俱进化工有限公司 The purifying technique and its equipment of a kind of lithium dodecyl sulfate
CN110092729A (en) * 2019-05-31 2019-08-06 上海泰坦科技股份有限公司 A kind of method for crystallising of L lysine HCL

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101558164A (en) * 2006-12-25 2009-10-14 味之素株式会社 Method of obtaining crystal of hydrochloride of basic amino acid
RU2410435C1 (en) * 2009-05-22 2011-01-27 Государственное образовательное учреждение высшего профессионального образования "Московский государственный университет инженерной экологии", МГУИЭ Method of extracting l-lysine from culture fluid
CN102875404A (en) * 2012-10-12 2013-01-16 中粮生物化学(安徽)股份有限公司 Production method and application of lysine hydrochloride crystals
CN103724218A (en) * 2014-01-22 2014-04-16 呼伦贝尔东北阜丰生物科技有限公司 New crystallization technology of lysine hydrochloride
CN103739507A (en) * 2013-10-08 2014-04-23 蚌埠丰原医药科技发展有限公司 Preparation method of beta-crystal-form lysine hydrochloride

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101558164A (en) * 2006-12-25 2009-10-14 味之素株式会社 Method of obtaining crystal of hydrochloride of basic amino acid
RU2410435C1 (en) * 2009-05-22 2011-01-27 Государственное образовательное учреждение высшего профессионального образования "Московский государственный университет инженерной экологии", МГУИЭ Method of extracting l-lysine from culture fluid
CN102875404A (en) * 2012-10-12 2013-01-16 中粮生物化学(安徽)股份有限公司 Production method and application of lysine hydrochloride crystals
CN103739507A (en) * 2013-10-08 2014-04-23 蚌埠丰原医药科技发展有限公司 Preparation method of beta-crystal-form lysine hydrochloride
CN103724218A (en) * 2014-01-22 2014-04-16 呼伦贝尔东北阜丰生物科技有限公司 New crystallization technology of lysine hydrochloride

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* Cited by examiner, † Cited by third party
Title
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105503630A (en) * 2015-12-04 2016-04-20 安徽丰原发酵技术工程研究有限公司 Method for purifying lysine hydrochloride
CN107501137A (en) * 2017-08-29 2017-12-22 东明俱进化工有限公司 The purifying technique and its equipment of a kind of lithium dodecyl sulfate
CN107501137B (en) * 2017-08-29 2023-09-05 东明俱进化工有限公司 Purification process and equipment for lithium dodecyl sulfate
CN110092729A (en) * 2019-05-31 2019-08-06 上海泰坦科技股份有限公司 A kind of method for crystallising of L lysine HCL
CN110092729B (en) * 2019-05-31 2022-06-28 上海泰坦科技股份有限公司 Crystallization method of L-lysine hydrochloride

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Application publication date: 20150909