CN107699918B - A kind of production technology of L-cysteine hydrochloride - Google Patents
A kind of production technology of L-cysteine hydrochloride Download PDFInfo
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- CN107699918B CN107699918B CN201710817437.8A CN201710817437A CN107699918B CN 107699918 B CN107699918 B CN 107699918B CN 201710817437 A CN201710817437 A CN 201710817437A CN 107699918 B CN107699918 B CN 107699918B
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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
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Abstract
The invention discloses a kind of production technologies of L-cysteine hydrochloride, belong to chemical process technical field；The technique comprises the steps of: a, prepares l-cysteine hydrochloric acid solution；B, it send the cathode chamber to electrolytic cell to be electrolysed l-cysteine hydrochloric acid solution, terminates electrolysis after the optical activity of electrolysis to cathode chamber solution is stablized；C, the feed liquid after electrolysis is concentrated, crystallized, obtain L-cysteine hydrochloride product crystal and mother liquor through being separated by solid-liquid separation；D, in the electrolytic process of step b, the mother liquor of step c is sent into electric tank cathode room, being mixed after common electrolysis is stablized to optical activity with cathode chamber solution terminates electrolysis；The present invention realizes the recycling of each batch mother liquor by the technique, the yield of L-cysteine hydrochloride product can be effectively improved, conducive to the stabilization of each batch quality, whole process discharging of waste liquid is few, simultaneously the process mother liquor using at low cost, high-efficient, circular economy is good.
Description
Technical field
The present invention relates to a kind of production technologies of L-cysteine hydrochloride, belong to chemical process technical field.
Background technique
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 mainstream production technology of L-cysteine hydrochloride, is by the way that l-cysteine hydrochloric acid solution is electric
Solution, concentration, crystallization are made.A kind of mode that is individually electrolysed again of post mother liquor that will crystallize is disclosed in CN1260409A carries out mother liquor
The technique of recycling is concentrated, crystallization processes again compared to mother liquor, effectively raises mother liquor product quality and product always recycles
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, affect the economy of process to a certain extent, also affect
Total yield of products.
Summary of the invention
Goal of the invention of the invention is: in view of the above problems, providing a kind of life of L-cysteine hydrochloride
Production. art redesigns the process route of disposing mother liquor, to improve the quality and overall recovery of product L-cysteine hydrochloride,
And improve the economy of process.
The technical solution adopted by the invention is as follows:
A kind of production technology of L-cysteine hydrochloride comprising the steps of:
A, l-cysteine hydrochloric acid solution is prepared；
B, the cathode chamber to electrolytic cell is sent to be electrolysed l-cysteine hydrochloric acid solution, when the rotation of electrolysis to cathode chamber solution
Luminosity terminates electrolysis after stablizing；
C, the feed liquid after electrolysis is concentrated, crystallized, obtain L-cysteine hydrochloride product crystal through being separated by solid-liquid separation
And mother liquor；
D, it repeats the above steps, in the electrolytic process of step b, the mother liquor of step c is sent into electric tank cathode room, with yin
The common electrolysis of pole room solution mixing terminates electrolysis after stablizing to optical activity.
Further, in the step a, the Baume degrees of the l-cysteine hydrochloric acid solution of preparation is 15-17 ° of Be'.
Further, in the step a, the Baume degrees of the l-cysteine hydrochloric acid solution of preparation is 16 ° of Be'.
It further, further include cleaning to prepared l-cysteine hydrochloric acid solution in the step a.
Further, in the step a, dedoping step includes activated carbon adsorption 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 one of nitric acid, hydrochloric acid, 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, it in the step b, 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.
It further, further include the decoloration before concentration to feed liquid after electrolysis in the step c.
Further, the decolorization includes activated carbon adsorption and filtering.
Further, feed liquid temperature, which is controlled, in the step c, in concentration process is not more than 80 DEG C.
Further, in the step c, use negative pressure concentration to control feed liquid temperature.
Further, in the step c, when concentration is completed, the Baume degrees of concentrate is 31-32 ° of Be'.
It further, further include the drying to L-cysteine hydrochloride product crystal in the step c.
Further, the L-cysteine hydrochloride product crystal uses low temperature drying.
Further, in the step c, the diluted acid of concentration process evaporation is recycled.
Further, the diluted acid that the concentration process recycles is used for the preparation of l-cysteine hydrochloric acid solution.
Further, in the step d, in the electrolytic process of step b, when the optical activity of cathode chamber solution is from left-handed change
Change to when dextrorotation, the mother liquor of step c is sent into electric tank cathode room, common electrolysis to optical activity is mixed with cathode chamber solution and is stablized
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 conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are: electrolytic cell yin is added in mother liquor
Pole room and l-cysteine hydrochloric acid solution form mixed solution, and mixed solution is continued to be electrolysed, and by the technological design, realize each
The recycling of batch mother liquor can effectively improve half Guang of L- compared to the mode that individually mother liquor is electrolysed or is recrystallized
The yield of propylhomoserin hydrochloric acid product salt, each batch quality is stablized, and whole process discharging of waste liquid is few, while individually electric compared to mother liquor
Solution, the process mother liquor using at low cost, high-efficient, circular economy is good.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
Any feature disclosed in this specification unless specifically stated can be equivalent or with similar purpose by other
Alternative features are replaced.That is, unless specifically stated, each feature is an example in a series of equivalent or similar characteristics
?.
The production technology of L-cysteine hydrochloride of the invention comprising the steps of:
A, l-cysteine hydrochloric acid solution is prepared；
B, the cathode chamber to electrolytic cell is sent to be electrolysed l-cysteine hydrochloric acid solution, when the rotation of electrolysis to cathode chamber solution
Luminosity terminates electrolysis after stablizing；
C, the feed liquid after electrolysis is concentrated, crystallized, obtain L-cysteine hydrochloride product crystal through being separated by solid-liquid separation
And mother liquor；
D, it repeats the above steps, in the electrolytic process of step b, the mother liquor of last step c is sent into electric tank cathode
Room, being mixed after common electrolysis is stablized to optical activity with this cathode chamber solution terminates electrolysis.
In the electrolytic process of l-cysteine hydrochloric acid solution, the optical activity of cathode chamber solution is gradually changed from left-handed to the right side
Rotation, and as the carry out dextrorotation value of electrolysis gradually increases, dextrorotation value to reach to peak value and relatively stable certain time, the continued electrolysis right side
Rotation value will be fallen after rise.Optical activity, which is stablized, in step b refers to the cathode chamber solution dextrorotation value reach to peak value and relatively steady state.
Embodiment 1
The production technology of L-cysteine hydrochloride, passes through following steps:
A, using 1 ton of l-cysteine and suitable hydrochloric acid as raw material, l-cysteine hydrochloric acid solution is prepared, obtaining Baume degrees is
The l-cysteine hydrochloric acid solution of 15 ° of Be' is added suitable active carbon to the l-cysteine hydrochloric acid solution and carries out impurity absorption, mistake
Filter；
B, the cathode chamber to electrolytic cell is sent to be electrolysed l-cysteine hydrochloric acid solution, the solution of electrolyzer anode chamber is nitre
Acid, cathode electrode material are lead, and anode electrode material is that titanium plates iridium, are terminated after being electrolysed the optical activity to cathode chamber solution and stablizing
It is electrolysed, is electrolysed in electrolytic process using low-voltage, the high current of 500A of 50v；
C, the feed liquid after electrolysis is sent into bleacher, active carbon decoloring is added, then through plate-frame filtering, micropore filter element refined filtration
Afterwards, it send to concentration tank and is concentrated, use negative pressure concentration to control feed liquid temperature no more than 80 DEG C in concentration process, wave is obtained after concentration
U.S. degree is the concentrate of 31 ° of Be', concentrate is sent to cooling tank, stirring to room temperature makes concentrate crystallization completely, solid through centrifuge
The isolated wet product L-cysteine hydrochloride product crystal of liquid and mother liquor, L-cysteine hydrochloride product crystal is sent to rolling
Cylinder drier is dried at 60 DEG C to finished product, and mother liquor is spare；
D, repeat above-mentioned steps, wherein in the electrolytic process of step b, when cathode chamber solution in optical activity from left-handed
When being changed near dextrorotation, the mother liquor in last step c is sent into electric tank cathode room, it is mixed with this cathode chamber solution
Amounting to terminates electrolysis after stablizing with electrolysis to optical activity.
During the L-cysteine hydrochloride of present embodiment each batch, the mother liquor total volume of each step c meets yin
The requirement of pole room liquor capacity 10-30% realizes whole circulations of each mother liquor and utilizes, through 35 Recycling Mother Solutions, mother liquor
It is no longer recycled, can mother liquor be individually electrolysed or be carried out subsequent processing utilization.
In the present embodiment, each batch finished product is the bar shaped granular crystals of clear, colorless, is detected as half Guang ammonia of L-
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 stable product quality of each batch.
Embodiment 2
The production technology of L-cysteine hydrochloride, passes through following steps:
A, using 1 ton of l-cysteine and suitable hydrochloric acid as raw material, l-cysteine hydrochloric acid solution is prepared, obtaining Baume degrees is
The l-cysteine hydrochloric acid solution of 16 ° of Be' is added suitable active carbon to the l-cysteine hydrochloric acid solution and carries out impurity absorption, mistake
Filter；
B, the cathode chamber to electrolytic cell is sent to be electrolysed l-cysteine hydrochloric acid solution, the solution of electrolyzer anode chamber is nitre
Acid, cathode electrode material are lead, and anode electrode material is that titanium plates iridium, are terminated after being electrolysed the optical activity to cathode chamber solution and stablizing
It is electrolysed, is electrolysed in electrolytic process using low-voltage, the high current of 250A of 100v；
C, the feed liquid after electrolysis is sent into bleacher, active carbon decoloring is added, then through plate-frame filtering, micropore filter element refined filtration
Afterwards, it send to concentration tank and is concentrated, use negative pressure concentration to control feed liquid temperature no more than 80 DEG C in concentration process, wave is obtained after concentration
U.S. degree is the concentrate of 32 ° of Be', concentrate is sent to cooling tank, stirring to room temperature makes concentrate crystallization completely, solid through centrifuge
The isolated wet product L-cysteine hydrochloride product crystal of liquid and mother liquor, L-cysteine hydrochloride product crystal is sent to rolling
Cylinder drier is dried at 60 DEG C to finished product, and mother liquor is spare；
D, repeat above-mentioned steps, wherein in the electrolytic process of step b, when cathode chamber solution in optical activity just from a left side
When rotation is changed to dextrorotation, the mother liquor of step c in the last time is sent into electric tank cathode room, is mixed jointly with this cathode chamber solution
Electrolysis terminates electrolysis after stablizing to optical activity.
During the L-cysteine hydrochloride of present embodiment each batch, the mother liquor total volume of each step c meets yin
The requirement of pole room liquor capacity 10-30% realizes whole circulations of each mother liquor and utilizes, through 32 Recycling Mother Solutions, mother liquor
It is no longer recycled, can mother liquor be individually electrolysed or be carried out subsequent processing utilization.
In the present embodiment, each batch finished product is the bar shaped granular crystals of clear, colorless, is detected as half Guang ammonia of L-
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 stable product quality of each batch.
Embodiment 3
The production technology of L-cysteine hydrochloride, passes through following steps:
It a, include the diluted acid recycled in step c concentration process in the hydrochloric acid using l-cysteine and suitable hydrochloric acid as raw material,
L-cysteine hydrochloric acid solution is prepared, the l-cysteine hydrochloric acid solution that Baume degrees is 17 ° of Be' is obtained, it is molten to the l-cysteine hydrochloric acid
Liquid is added suitable active carbon and carries out impurity absorption, filtering；
B, the cathode chamber to electrolytic cell is sent to be electrolysed l-cysteine hydrochloric acid solution, the solution of electrolyzer anode chamber is nitre
Acid, cathode electrode material are lead, and anode electrode material is that titanium plates iridium, are terminated after being electrolysed the optical activity to cathode chamber solution and stablizing
It is electrolysed, is electrolysed in electrolytic process using low-voltage, the high current of 250A of 100v；
C, the feed liquid after electrolysis is sent into bleacher, active carbon decoloring is added, then through plate-frame filtering, micropore filter element refined filtration
Afterwards, it send to concentration tank and is concentrated, use negative pressure concentration to control feed liquid temperature no more than 80 DEG C in concentration process, steamed in concentration process
The diluted acid of hair is recycled, and the concentrate that Baume degrees is 32 ° of Be' is obtained after concentration, and concentrate is sent to cooling tank, is stirred to normal
Temperature makes concentrate crystallization completely, is separated by solid-liquid separation to obtain wet product L-cysteine hydrochloride product crystal and mother liquor through centrifuge, will
L-cysteine hydrochloride product crystal is sent to drum dryer and is dried at 60 DEG C to finished product, and mother liquor is spare；
D, repeat above-mentioned steps, wherein in the electrolytic process of step b, when cathode chamber solution in optical activity just from a left side
When rotation is changed to dextrorotation, the mother liquor of step c in the last time is sent into electric tank cathode room, is mixed jointly with this cathode chamber solution
Electrolysis terminates electrolysis after stablizing to optical activity.
During the L-cysteine hydrochloride of present embodiment each batch, the mother liquor total volume of each step c meets yin
The requirement of pole room liquor capacity 10-30% realizes whole circulations of each mother liquor and utilizes, through 30 Recycling Mother Solutions, mother liquor
It is no longer recycled, can mother liquor be individually electrolysed or be carried out subsequent processing utilization.
In the present embodiment, each batch finished product is the bar shaped granular crystals of clear, colorless, is detected as half Guang ammonia of L-
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 stable product quality of each batch.
Embodiment 4
The embodiment and embodiment 1, implementation 2, embodiment 3 are essentially identical, except that in step d: being will be last
After the mother liquor feeding electric tank cathode room of middle step c is mixed with this cathode chamber solution, then start to be electrolysed, electrolysis to optically-active
Degree terminates electrolysis after stablizing；Either after electrolysis starts, the mother of step c is added when optical activity is left-handed for cathode chamber solution
Liquid, electrolysis to optical activity terminate electrolysis after stablizing.
The embodiment the result shows that, each batch finished product be clear, colorless bar shaped granular crystals, through detecting
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 stablized, and the total recovery of single product is slightly lower 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 l-cysteine hydrochloric acid solution
It is electrolysed jointly, but mother liquor is subjected to independent electrolysis, concentration, crystallization, to achieve the purpose that mother liquor gives off system.
In the various embodiments described above, the acid solution of anode chamber be can also be one of hydrochloric acid, sulfuric acid or mixing.Electrolytic cell
Cathode electrode material can also for silver or copper it is silver-plated, anode electrode material can also be carbon plate.
This technique has following remarkable advantage: (1) being carried out by the feed liquid after l-cysteine concentration of hydrochloric acid solution, electrolysis dense
The control of contracting, enable the mother liquor of step c be all added to during step b mixed with l-cysteine hydrochloric acid solution simultaneously into
Row electrolysis；(2) mother liquor is recycled every time is electrolysed simultaneously with l-cysteine hydrochloric acid solution, compared to independent electrolytic process, tool
Have and do not occupy equipment progress individually, individually time-consuming the advantages of carrying out, the utilization efficiency of mother liquor are 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 efficiency of raising mother liquor, and guarantee the stabilization of each batch quality in mother liquor recycling；(4) mother liquor recycled
Journey is conducive to the abundant recycling of mother liquor, further improves total recovery；(5) entirely the discharge of circulation production process is few, produces
Cheng Huanbao, cleaning.
In the present invention, electric tank cathode room is added in mother liquor and l-cysteine hydrochloric acid solution forms mixed 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, and each batch quality is stablized, and whole
A process waste discharge is few, while being individually electrolysed compared to mother liquor, which utilizes at low cost, high-efficient, circular economy
Property is good.
The invention is not limited to specific embodiments above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (9)
1. a kind of production technology of L-cysteine hydrochloride, it is characterised in that: comprise the steps of:
A, l-cysteine hydrochloric acid solution is prepared；
B, the cathode chamber to electrolytic cell is sent to be electrolysed l-cysteine hydrochloric acid solution, when the optical activity of electrolysis to cathode chamber solution
Terminate electrolysis after stabilization；
C, the feed liquid after electrolysis is concentrated, crystallized, obtain L-cysteine hydrochloride product crystal and mother through being separated by solid-liquid separation
Liquid；
D, in the electrolytic process of step b, when the optical activity of cathode chamber solution from it is left-handed be changed to dextrorotation when, by the mother of step c
Liquid is sent into electric tank cathode room, and being mixed after common electrolysis is stablized to optical activity with cathode chamber solution terminates electrolysis.
2. the production technology of L-cysteine hydrochloride as described in claim 1, it is characterised in that: in the step a, prepare
L-cysteine hydrochloric acid solution Baume degrees be 15-17 ° of Be'.
3. the production technology of L-cysteine hydrochloride as described 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 described in claim 1, it is characterised in that: in the step b, electrolysis
The cathode electrode material of slot 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 described 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 described in claim 1, it is characterised in that: in the step c, concentration
Control feed liquid temperature is not more than 80 DEG C in the process.
7. the production technology of L-cysteine hydrochloride as described in claim 1, it is characterised in that: in the step c, concentration
When completion, the Baume degrees of concentrate is 31-32 ° of Be'.
8. the production technology of L-cysteine hydrochloride as described in claim 1, it is characterised in that: in the step c, to dense
The diluted acid of compression process evaporation is recycled.
9. the production technology of L-cysteine hydrochloride as described in claim 1, it is characterised in that: in the step d, mother liquor
Addition volume be cathode chamber solution volume 10-30%.
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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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