CN107699918A - A kind of production technology of L cysteine hydrochlorides - Google Patents
A kind of production technology of L cysteine hydrochlorides Download PDFInfo
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- CN107699918A CN107699918A CN201710817437.8A CN201710817437A CN107699918A CN 107699918 A CN107699918 A CN 107699918A CN 201710817437 A CN201710817437 A CN 201710817437A CN 107699918 A CN107699918 A CN 107699918A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/25—Reduction
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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Abstract
The invention discloses a kind of production technology of L cysteine hydrochlorides, belong to chemical process technical field；The technique comprises the steps of：A, L cystine salt acid solutions are prepared；The cathode chamber that L cystine salt acid solutions are delivered to electrolytic cell is electrolysed b, terminates electrolysis after the optical activity of electrolysis to cathode chamber solution is stable；C, the feed liquid after electrolysis is concentrated, crystallized, L cysteine hydrochlorides product crystal and mother liquor are obtained through separation of solid and liquid；D, in step b electrolytic process, step c mother liquor is sent into electric tank cathode room, terminates electrolysis after common electrolysis to optical activity stabilization is mixed with cathode chamber solution；The present invention realizes the recycling of each batch mother liquor by the technique, the yield of L cysteine hydrochloride products can be effectively improved, it is few beneficial to the stabilization of each batch quality, whole process discharging of waste liquid, while the utilization cost of the process mother liquor is low, efficiency high, recycling economy is good.
Description
Technical field
The present invention relates to a kind of production technology of L-cysteine hydrochloride, belong to chemical process technical field.
Background technology
L-cysteine hydrochloride has a wide range of applications in food, medicine and other fields, is a kind of important amino acid.
Electrolytic reduction is the main flow production technology of L-cysteine hydrochloride, is by the way that CYSTINE hydrochloric acid solution is electric
Solution, concentration, crystallization are made.A kind of mode for being individually electrolysed crystallization Mother liquor again is disclosed in CN1260409A and carries out mother liquor
The technique of recovery, concentrated again compared to mother liquor, crystallization processes, effectively raise mother liquor product quality and product always reclaims
Rate.Although the mother liquor in CN1260409A is individually electrolysed again improves total recovery to a certain extent, electrolytic process consumption
Duration, mother liquid disposal amount are small, mother liquor discards the high factor of rate, have impact on the economy of process to a certain extent, also have impact on
Total yield of products.
The content of the invention
The goal of the invention of the present invention is：For above-mentioned problem, there is provided a kind of life of L-cysteine hydrochloride
Production. art, the process route of disposing mother liquor is redesigned, to improve the quality of product L-cysteine hydrochloride and overall recovery,
And improve the economy of process.
The technical solution adopted by the present invention is as follows：
A kind of production technology of L-cysteine hydrochloride, is comprised the steps of：
A, CYSTINE hydrochloric acid solution is prepared；
The cathode chamber that CYSTINE hydrochloric acid solution is delivered to electrolytic cell is electrolysed b, when the optical activity of electrolysis to cathode chamber solution
Terminate electrolysis after stable；
C, the feed liquid after electrolysis is concentrated, crystallized, L-cysteine hydrochloride product crystal and mother are obtained through separation of solid and liquid
Liquid；
D, repeat the above steps, in step b electrolytic process, step c mother liquor is sent into electric tank cathode room, with cathode chamber
Terminate electrolysis after the common electrolysis of solution mixing to optical activity stabilization.
Further, in the step a, the Baume degrees of the CYSTINE hydrochloric acid solution of preparation is 15-17 ° of Be'.
Further, in the step a, the Baume degrees of the CYSTINE hydrochloric acid solution of preparation is 16 ° of Be'.
Further, in the step a, in addition to the CYSTINE hydrochloric acid solution to being prepared cleans.
Further, in the step a, dedoping step includes charcoal absorption and filtering.
Further, in the step b, the solution of anode chamber is acid solution.
Further, in the step b, the acid solution of anode chamber is nitric acid, hydrochloric acid, one kind in sulfuric acid or mixing.
Further, in the step b, the acid solution of anode chamber is nitric acid.
Further, in the step b, the cathode electrode material of electrolytic cell is that lead, silver or copper are silver-plated, anode electrode material
Iridium or carbon plate are plated for titanium.
Further, in the step b, the cathode electrode material of electrolytic cell is lead, and anode electrode material is that titanium plates iridium.
Further, in the step b, it is electrolysed using low-voltage, high current.
Further, in the step b, the voltage of electrolysis is 50v-100v, and electric current is 500A -250A.
Further, in the step c, it is additionally included in the decolouring to feed liquid after electrolysis before concentration.
Further, the decolorization includes charcoal absorption and filtering.
Further, in the step c, feed temperature is controlled to be not more than 80 DEG C in concentration process.
Further, in the step c, negative pressure concentration is used to control feed temperature.
Further, in the step c, when concentration is completed, the Baume degrees of concentrate is 31-32 ° of Be'.
Further, in the step c, in addition to the drying to L-cysteine hydrochloride product crystal.
Further, the L-cysteine hydrochloride product crystal uses low temperature drying.
Further, in the step c, the diluted acid of concentration process evaporation is reclaimed.
Further, the diluted acid concentration process reclaimed is used for the preparation of CYSTINE hydrochloric acid solution.
Further, in the step d, in step b electrolytic process, when the optical activity of cathode chamber solution is from left-handed change
Change to during dextrorotation, step c mother liquor is sent into electric tank cathode room, it is stable to optical activity that common electrolysis is mixed with cathode chamber solution
After terminate to be electrolysed.
Further, in the step d, mother liquor recycles number no more than 35 times.
Further, in the step d, the addition volume of mother liquor is the 10-30% of cathode chamber solution volume.
In summary, by adopting the above-described technical solution, the beneficial effects of the invention are as follows：It is cloudy that mother liquor is added into electrolytic cell
Pole room forms mixed solution with CYSTINE hydrochloric acid solution, and mixed solution is continued to be electrolysed, and by the technological design, realizes each
The recycling of batch mother liquor, compared to the mode that individually mother liquor is electrolysed or recrystallized, it can effectively improve the Guangs of L- half
The yield of propylhomoserin hydrochloric acid product salt, each batch steady quality, and whole process discharging of waste liquid is few, at the same it is individually electric compared to mother liquor
Solution, the utilization cost of the process mother liquor is low, efficiency high, and recycling economy is good.
Embodiment
All features disclosed in this specification, or disclosed all methods or during the step of, except mutually exclusive
Feature and/or step beyond, can combine in any way.
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent by other or with similar purpose
Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics
.
The production technology of the L-cysteine hydrochloride of the present invention, is comprised the steps of：
A, CYSTINE hydrochloric acid solution is prepared；
The cathode chamber that CYSTINE hydrochloric acid solution is delivered to electrolytic cell is electrolysed b, when the optical activity of electrolysis to cathode chamber solution
Terminate electrolysis after stable；
C, the feed liquid after electrolysis is concentrated, crystallized, L-cysteine hydrochloride product crystal and mother are obtained through separation of solid and liquid
Liquid；
D, repeat the above steps, in step b electrolytic process, last step c mother liquor is sent into electric tank cathode room, with
Terminate electrolysis after this common electrolysis of cathode chamber solution mixing to optical activity stabilization.
In the electrolytic process of CYSTINE hydrochloric acid solution, the optical activity of cathode chamber solution is gradually changed to the right side from left-handed
Rotation, and gradually increase with the carry out dextrorotation value of electrolysis, dextrorotation value to peaking and relatively stable certain time, the continued electrolysis right side
Rotation value will fall after rise.Optical activity is stable in step b refers to the cathode chamber solution dextrorotation value peaking and relatively steady state.
Embodiment 1
The production technology of L-cysteine hydrochloride, passes through following steps：
A, using 1 ton of CYSTINE and appropriate hydrochloric acid as raw material, CYSTINE hydrochloric acid solution is prepared, it is 15 ° of Be' to obtain Baume degrees
CYSTINE hydrochloric acid solution, add appropriate activated carbon to the CYSTINE hydrochloric acid solution and carry out impurity absorption, filtering；
The cathode chamber that CYSTINE hydrochloric acid solution is delivered to electrolytic cell is electrolysed b, and the solution of electrolyzer anode chamber is nitric acid,
Cathode electrode material is lead, and anode electrode material is that titanium plates iridium, terminates electricity after the optical activity of electrolysis to cathode chamber solution is stable
Solve, be electrolysed in electrolytic process using 50v low-voltage, 500A high current；
C, the feed liquid after electrolysis is sent into bleacher, adds activated carbon decolorizing, then after plate-frame filtering, micropore filter element refined filtration, send
Concentrated to concentration tank, use negative pressure concentration to obtain Baume degrees after concentration to control feed temperature to be not more than 80 DEG C in concentration process
For 31 ° of Be' concentrate, concentrate is delivered into cooling tank, stirring to normal temperature makes concentrate crystallization complete, through centrifuge solid-liquid point
From wet product L-cysteine hydrochloride product crystal and mother liquor is obtained, L-cysteine hydrochloride product crystal is delivered into roller and done
The drying at 60 DEG C of dry device is standby to finished product, mother liquor；
D, above-mentioned steps are repeated, wherein in step b electrolytic process, when cathode chamber solution in optical activity from left-handed change
When near to dextrorotation, the mother liquor in last step c is sent into electric tank cathode room, mixed with this cathode chamber solution altogether
With end electrolysis after electrolysis to optical activity stabilization.
During the L-cysteine hydrochloride of each batch of present embodiment, each step c mother liquor cumulative volume meets the moon
Pole room liquor capacity 10-30% requirement, realize whole circulations of each mother liquor and utilize, through the Recycling Mother Solution of 35 times, mother liquor
No longer recycled, mother liquor individually can be electrolysed or be carried out subsequent treatment utilization.
In the present embodiment, each batch finished product is the bar shaped granular crystals of clear, colorless, is detected as the Guang ammonia of L- half
Acid hydrochloride, product meet the standard of Japanese aginomoto, and the total recovery of product reaches 144%, in the cycle period of mother liquor,
The product quality of each batch is stable.
Embodiment 2
The production technology of L-cysteine hydrochloride, passes through following steps：
A, using 1 ton of CYSTINE and appropriate hydrochloric acid as raw material, CYSTINE hydrochloric acid solution is prepared, it is 16 ° of Be' to obtain Baume degrees
CYSTINE hydrochloric acid solution, add appropriate activated carbon to the CYSTINE hydrochloric acid solution and carry out impurity absorption, filtering；
The cathode chamber that CYSTINE hydrochloric acid solution is delivered to electrolytic cell is electrolysed b, and the solution of electrolyzer anode chamber is nitric acid,
Cathode electrode material is lead, and anode electrode material is that titanium plates iridium, terminates electricity after the optical activity of electrolysis to cathode chamber solution is stable
Solve, be electrolysed in electrolytic process using 100v low-voltage, 250A high current；
C, the feed liquid after electrolysis is sent into bleacher, adds activated carbon decolorizing, then after plate-frame filtering, micropore filter element refined filtration, send
Concentrated to concentration tank, use negative pressure concentration to obtain Baume degrees after concentration to control feed temperature to be not more than 80 DEG C in concentration process
For 32 ° of Be' concentrate, concentrate is delivered into cooling tank, stirring to normal temperature makes concentrate crystallization complete, through centrifuge solid-liquid point
From wet product L-cysteine hydrochloride product crystal and mother liquor is obtained, L-cysteine hydrochloride product crystal is delivered into roller and done
The drying at 60 DEG C of dry device is standby to finished product, mother liquor；
D, above-mentioned steps are repeated, wherein in step b electrolytic process, when cathode chamber solution in optical activity just from left-handed change
Change to during dextrorotation, the mother liquor of step c in the last time is sent into electric tank cathode room, common electrolysis is mixed with this cathode chamber solution
Terminate electrolysis after to optical activity stabilization.
During the L-cysteine hydrochloride of each batch of present embodiment, each step c mother liquor cumulative volume meets the moon
Pole room liquor capacity 10-30% requirement, realize whole circulations of each mother liquor and utilize, through the Recycling Mother Solution of 32 times, mother liquor
No longer recycled, mother liquor individually can be electrolysed or be carried out subsequent treatment utilization.
In the present embodiment, each batch finished product is the bar shaped granular crystals of clear, colorless, is detected as the Guang ammonia of L- half
Acid hydrochloride, product meet the standard of Japanese aginomoto, and the total recovery of product reaches 144%, in the cycle period of mother liquor,
The product quality of each batch is stable.
Embodiment 3
The production technology of L-cysteine hydrochloride, passes through following steps：
A, the diluted acid reclaimed in step c concentration process is included using CYSTINE and appropriate hydrochloric acid as raw material, in the hydrochloric acid, is prepared
CYSTINE hydrochloric acid solution, CYSTINE hydrochloric acid solution of the Baume degrees for 17 ° of Be' is obtained, is added to the CYSTINE hydrochloric acid solution
Enter appropriate activated carbon and carry out impurity absorption, filtering；
The cathode chamber that CYSTINE hydrochloric acid solution is delivered to electrolytic cell is electrolysed b, and the solution of electrolyzer anode chamber is nitric acid,
Cathode electrode material is lead, and anode electrode material is that titanium plates iridium, terminates electricity after the optical activity of electrolysis to cathode chamber solution is stable
Solve, be electrolysed in electrolytic process using 100v low-voltage, 250A high current；
C, the feed liquid after electrolysis is sent into bleacher, adds activated carbon decolorizing, then after plate-frame filtering, micropore filter element refined filtration, send
Concentrated to concentration tank, use negative pressure concentration to be evaporated to control feed temperature to be not more than 80 DEG C in concentration process in concentration process
Diluted acid is reclaimed, and concentrate of the Baume degrees for 32 ° of Be' is obtained after concentration, concentrate is delivered into cooling tank, stirring to normal temperature makes
Concentrate crystallization is complete, and wet product L-cysteine hydrochloride product crystal and mother liquor are obtained through centrifuge separation of solid and liquid, by L- half
It is standby to finished product, mother liquor that cystine hydrochloride product crystal delivers to drum dryer drying at 60 DEG C；
D, above-mentioned steps are repeated, wherein in step b electrolytic process, when cathode chamber solution in optical activity just from left-handed change
Change to during dextrorotation, the mother liquor of step c in the last time is sent into electric tank cathode room, common electrolysis is mixed with this cathode chamber solution
Terminate electrolysis after to optical activity stabilization.
During the L-cysteine hydrochloride of each batch of present embodiment, each step c mother liquor cumulative volume meets the moon
Pole room liquor capacity 10-30% requirement, realize whole circulations of each mother liquor and utilize, through the Recycling Mother Solution of 30 times, mother liquor
No longer recycled, mother liquor individually can be electrolysed or be carried out subsequent treatment utilization.
In the present embodiment, each batch finished product is the bar shaped granular crystals of clear, colorless, is detected as the Guang ammonia of L- half
Acid hydrochloride, product meet the standard of Japanese aginomoto, and the total recovery of product reaches 144%, in the cycle period of mother liquor,
The product quality of each batch is stable.
Embodiment 4
The embodiment and embodiment 1, implementation 2, embodiment 3 are essentially identical, except that in step d：It is that will be walked in the last time
After rapid c mother liquor feeding electric tank cathode room mixes with this cathode chamber solution, then electrolysis is proceeded by, be electrolysed steady to optical activity
Terminate electrolysis after fixed；Either after electrolysis starts, cathode chamber solution adds step c mother liquor, electricity when optical activity is left-handed
Terminate electrolysis after solution to optical activity stabilization.
The result of the embodiment shows that each batch finished product is the bar shaped granular crystals of clear, colorless, after testing
For L-cysteine hydrochloride, product meets the standard of Japanese aginomoto, in the cycle period of mother liquor, the product matter of each batch
Amount is stable, and the total recovery of single product is lower slightly compared to embodiment 1, implementation 2, embodiment 3, but is greatly higher than and individually carries out mother liquor electricity
The total recovery of solution, while the energy consumption of production process is slightly larger than embodiment 1, implementation 2, embodiment 3.
In the various embodiments described above, as the increase of the recycling number of mother liquor may cause the accumulation of impurity, work as mother liquor
Cycle-index reach 35 times when, there is greater probability to have an impact the quality of product, mother liquor no longer with CYSTINE hydrochloric acid solution
It is electrolysed jointly, but mother liquor is subjected to independent electrolysis, concentration, crystallization, reaches the purpose that mother liquor gives off system.
In the various embodiments described above, it can also be one kind or mixing in hydrochloric acid, sulfuric acid that the acid solution of anode chamber, which is,.Electrolytic cell
Cathode electrode material can also be silver or copper it is silver-plated, anode electrode material can also be carbon plate.
This technique has following remarkable advantage：（1）Carried out by the feed liquid after CYSTINE concentration of hydrochloric acid solution, electrolysis dense
The control of contracting so that step c mother liquor can all be added to during step b and mix while enter with CYSTINE hydrochloric acid solution
Row electrolysis；（2）Recycling mother liquor every time is and CYSTINE hydrochloric acid solution while is electrolysed, and compared to independent electrolytic process, has
Have and do not take equipment progress individually, do not take the advantages of carrying out individually, the utilization ratio of mother liquor is high；（3）When cathode chamber solution
Optical activity from it is left-handed be changed to dextrorotation when, mother liquor is sent into electric tank cathode room mix with cathode chamber solution and be electrolysed jointly, favorably
In the utilization ratio of raising mother liquor, and ensure the stabilization of each batch quality in mother liquor recycling；（4）Mother liquor recycled
Journey, be advantageous to the abundant recovery of mother liquor, further improve total recovery；（5）The discharge of whole circulation production process is lacked, and produces
Cheng Huanbao, cleaning.
In the present invention, mother liquor is added into electric tank cathode room and forms mixed solution with CYSTINE hydrochloric acid solution, will be mixed
Solution continues to be electrolysed, and by the technological design, realizes the recycling of each batch mother liquor, compared to individually to mother liquor electrolysis or
The mode recrystallized, can effectively improve the yield of L-cysteine hydrochloride product, each batch steady quality, and whole
The discharge of individual process waste is few, while is individually electrolysed compared to mother liquor, and the utilization cost of the process mother liquor is low, efficiency high, recycling economy
Property is good.
The invention is not limited in foregoing embodiment.The present invention, which expands to, any in this manual to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (10)
- A kind of 1. production technology of L-cysteine hydrochloride, it is characterised in that：Comprise the steps of：A, CYSTINE hydrochloric acid solution is prepared；The cathode chamber that CYSTINE hydrochloric acid solution is delivered to electrolytic cell is electrolysed b, when the optical activity of electrolysis to cathode chamber solution Terminate electrolysis after stable；C, the feed liquid after electrolysis is concentrated, crystallized, L-cysteine hydrochloride product crystal and mother are obtained through separation of solid and liquid Liquid；D, in step b electrolytic process, step c mother liquor is sent into electric tank cathode room, mixed with cathode chamber solution jointly Terminate electrolysis after electrolysis to optical activity stabilization.
- 2. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step a, prepare The Baume degrees of CYSTINE hydrochloric acid solution be 15-17 ° of Be'.
- 3. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step b, anode The solution of room is acid solution.
- 4. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step b, electrolysis The cathode electrode material of groove is that lead, silver or copper are silver-plated, and anode electrode material is that titanium plates iridium or carbon plate.
- 5. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step b, use Low-voltage, high current are electrolysed.
- 6. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step c, concentration During control feed temperature be not more than 80 DEG C.
- 7. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step c, concentration During completion, the Baume degrees of concentrate is 31-32 ° of Be'.
- 8. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step c, to dense The diluted acid of compression process evaporation is reclaimed.
- 9. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：In the step d, in step In rapid b electrolytic process, when cathode chamber solution optical activity from it is left-handed be changed to dextrorotation when, step c mother liquor is sent into electrolysis Groove cathode chamber, terminate electrolysis after common electrolysis to optical activity stabilization is mixed with cathode chamber solution.
- 10. the production technology of L-cysteine hydrochloride as claimed in claim 1, it is characterised in that：It is female in the step d The addition volume of liquid is the 10-30% of cathode chamber solution volume.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110344077A (en) * | 2019-07-01 | 2019-10-18 | 吉林大学 | A method of by l-cysteine electrochemistry formated n-acetyl-L-cysteine |
| CN111118531A (en) * | 2019-12-31 | 2020-05-08 | 宁波市远发生物工程有限公司 | Preparation method of L-cysteine hydrochloride monohydrate |
| CN114855194A (en) * | 2022-06-12 | 2022-08-05 | 吉林大学 | Green production process of N-acetyl-L-cysteine |
| CN115772104A (en) * | 2022-11-15 | 2023-03-10 | 广东百澳药业有限公司 | Preparation method of N-acetyl-L-cysteine |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110344077A (en) * | 2019-07-01 | 2019-10-18 | 吉林大学 | A method of by l-cysteine electrochemistry formated n-acetyl-L-cysteine |
| CN111118531A (en) * | 2019-12-31 | 2020-05-08 | 宁波市远发生物工程有限公司 | Preparation method of L-cysteine hydrochloride monohydrate |
| CN114855194A (en) * | 2022-06-12 | 2022-08-05 | 吉林大学 | Green production process of N-acetyl-L-cysteine |
| CN115772104A (en) * | 2022-11-15 | 2023-03-10 | 广东百澳药业有限公司 | Preparation method of N-acetyl-L-cysteine |
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| Publication number | Publication date |
|---|---|
| CN107699918B (en) | 2019-07-02 |
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