CN106188189B - A kind of nucleosides acid mother liquor desalination and concentration method - Google Patents
A kind of nucleosides acid mother liquor desalination and concentration method Download PDFInfo
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- CN106188189B CN106188189B CN201610520997.2A CN201610520997A CN106188189B CN 106188189 B CN106188189 B CN 106188189B CN 201610520997 A CN201610520997 A CN 201610520997A CN 106188189 B CN106188189 B CN 106188189B
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- mother liquor
- nucleosides acid
- acid mother
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H19/00—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
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- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of nucleosides acid mother liquor desalination and concentration methods, it is specific as follows: (1) nucleosides acid mother liquor to be placed in batch can, start delivery pump, after nucleosides acid mother liquor is concentrated 2.5~5 times by membrane module, continue the continual addition water isometric with the amount of the permeate generated immediately into batch can as needed to continue to run, total amount of water is equal to the 65~75% of above-mentioned nucleosides acid mother liquor volume, and final positive and negative yield is all larger than 99%；The operating pressure of above equipment is 20~28bar, and temperature is 20~30 DEG C, and average flux is 12~30LMH；(2) then the residual liquid being rinsed with water in mold core and pipeline cleans 0.4~0.6h with cleaning solution under conditions of 30~40 DEG C, can restore mold core flux substantially.
Description
Technical field
The invention belongs to membrane technology fields, and in particular to a kind of nucleosides acid mother liquor desalination and concentration method.
Background technique
Nucleotide is almost to participate in cell as nucleic acid hydrolysis and through biological products obtained by further separation, concentration, drying
All biochemical processes.In the food industry, nucleotide is extended to have and improves organism via initial food fragrance adding agent
The functional food additives of immune function.Especially there is irreplaceable role in infant food, is mended in cow's milk
After having filled nucleotide, the milk replacer close to human milk, resistivity [2-3] of the enhancing baby to bacteriosis can be produced.This
Outside, nucleotide also has a wide range of applications in medicine, agricultural, fine chemistry industry.Therefore the large-scale production to nucleotide is realized,
With highly important social benefit and significant economic benefit.
Containing impurity such as a certain amount of phosphate anions in the existing nucleotide hydrolysis liquid produced by edman degradation Edman, at present
The method separating nucleotide of ion exchange resin and chromatography is generallyd use both at home and abroad, this method cannot be mass produced, and price
It is expensive.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of nucleosides acid mother liquor desalination and concentration method is provided.
The specific technical solution of the present invention is as follows:
A kind of nucleosides acid mother liquor desalination and concentration method, device therefor include passing sequentially through batch can that pipeline is connected, defeated
Pump, membrane module, pressure regulator valve and heat exchanger are sent, wherein the mold core of membrane module is 3B01 nanofiltration membrane, which has a concentrate
Outlet and permeate outlet, concentrated solution outlet is connected by pipeline with pressure regulator valve, the liquid outlet of heat exchanger pass through pipeline and
Batch can is connected,
This method is specific as follows:
(1) nucleosides acid mother liquor is placed in batch can, start delivery pump, by nucleosides acid mother liquor by membrane module be concentrated 2.8~
After 3.3 times, continues continual add into batch can as needed and continue with the isometric water of the amount of the permeate generated immediately
Operation, total amount of water are equal to the 70% of above-mentioned nucleosides acid mother liquor volume, and final Na removal rate is that 71~80%, Cl removal rate is
93.2~93.8%, 0.05g/L is lower than by the content of liquid nucleotide, positive and negative yield is all larger than 99%.；
(2) then the residual liquid being rinsed with water in mold core and pipeline is cleaned under conditions of 30~40 DEG C with cleaning solution
0.4~0.6h can restore mold core flux substantially.
In a preferred embodiment of the invention, the nucleosides acid mother liquor is nucleotide primary crystallization mother liquor (i.e. core
Liquid Residue of the thuja acid feed liquid after crystallization).
It is further preferred that the operating pressure of the equipment is 20~26bar, temperature is 20~26 DEG C, and average flux is
12~13.5LMH.
It is further preferred that the step (1) are as follows: nucleosides acid mother liquor is placed in batch can, starts delivery pump, by nucleotide
Mother liquor by membrane module be concentrated 2.8~3.3 times after, continue as needed it is continual into batch can addition with generate immediately it is saturating
The isometric water of amount for crossing liquid continues to run, and total amount of water is equal to the 70% of above-mentioned nucleosides acid mother liquor volume, final Na removal
Rate is that 71~80%, Cl removal rate is 93.2~93.8%, is lower than 0.05g/L, positive and negative yield by the content of liquid nucleotide
It is all larger than 99%.
In a preferred embodiment of the invention, the nucleosides acid mother liquor is nucleotide secondary crystallization mother liquor (i.e. core
Crystalline mother solution after thuja acid secondary crystallization is complete).
It is further preferred that the operating pressure of the equipment is 20~28bar, temperature is 23~30 DEG C, and average flux is
25~30LMH.
It is further preferred that the step (1) are as follows: nucleosides acid mother liquor is placed in batch can, starts delivery pump, by nucleotide
Mother liquor is concentrated 5 times by membrane module, and final anti-yield is greater than 99%.
The beneficial effects of the present invention are: method of the invention can effectively remove Na and Cl in nucleosides acid mother liquor, simultaneously
With the positive and negative yield for being greater than 99%, desalting effect is good, and is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of equipment of the invention.
Fig. 2 is the membrane flux curve graph of the embodiment of the present invention 1.
Fig. 3 is the membrane flux curve graph of the embodiment of the present invention 2.
Specific embodiment
Technical solution of the present invention is further explained and described below by way of specific embodiment combination attached drawing.
1 nucleotide primary crystallization mother liquor of embodiment stablizes experiment
As shown in Figure 1, the embodiment device therefor includes passing sequentially through batch can 1, the delivery pump 2, film group that pipeline is connected
Part 3, pressure regulator valve 4 and heat exchanger 5, wherein the mold core of membrane module 3 is 3B01 nanofiltration membrane, which has a concentrated solution outlet
It is exported with a permeate, concentrated solution outlet is connected by pipeline with pressure regulator valve 4, and the liquid outlet of heat exchanger 5 passes through pipeline and material
Tank 1 is connected,
This method is specific as follows:
(1) nucleotide primary crystallization mother liquor is placed in batch can 1, starts delivery pump 2, nucleotide primary crystallization mother liquor is led to
After crossing 2.5~5 times of the concentration of membrane module 3, continue the continual permeate added into batch can 1 and generated immediately as needed
It measures isometric water to continue to run, total amount of water is equal to the 65~75% of above-mentioned nucleotide primary crystallization mother liquor volume, finally
Positive and negative yield is all larger than 99%；The operating pressure of above equipment is 20~28bar, and temperature is 20~30 DEG C, average flux 12
~30LMH；The operating pressure of the equipment is 20~26bar, and temperature is 20~26 DEG C, and average flux is 12~13.5LMH；
(2) then the residual liquid being rinsed with water in mold core and pipeline is cleaned under conditions of 30~40 DEG C with cleaning solution
0.4~0.6h can restore mold core flux substantially.
By nucleotide primary crystallization mother liquor according to above-mentioned steps, carries out stablizing experiment, carried out 3 batches, every batch of in total
It is secondary that a certain amount of nucleotide primary crystallization mother liquor is taken to be tested, operating pressure control 20-25bar, temperature control 30 DEG C with
It is interior, 3 times or so are concentrated, amount of water is 2 times or so of concentrate, finally can achieve 80% or so, cl's to the removal rate of Na
Removal rate 93% or so, waste liquid nucleotide content are lower than 0.05g/L；Positive and negative yield is all larger than 99%；Detailed Experimental data are shown in
The following table 1, table 2 and Fig. 2:
Table 1: experiment operation data
Table 2: experimental test data
Analysis of experimental results
In running temperature control in 30 DEG C, is operated under conditions of operating pressure 20-26bar, be concentrated into 3 times of left sides
The right side, flux are reduced to 10LMH or so, start plus 2 times of volume of the concentrated liquid of water are eluted, and liquid waste residues content is lower than 0.02g/L,
Positive and negative yield is all larger than 99%；To the removal rate 80% or so of Na, the removal rate of cl is 93% or so；The operation of film core flux is opposite
Stablize, average flux reaches 12-13.5LMH；The variation of experimentation flux detector, meets film core moving law, in the initial stage
Feed concentration is relatively low, and flux is larger, begins to decline with concentration flux, and with water elution is added, flux slightly rises, directly
To tending towards stability.
2 nucleotide primary crystallization mother liquor of embodiment stablizes experiment
As shown in Figure 1, the embodiment device therefor includes passing sequentially through batch can 1, the delivery pump 2, film group that pipeline is connected
Part 3, pressure regulator valve 4 and heat exchanger 5, wherein the mold core of membrane module 3 is 3B01 nanofiltration membrane, which has a concentrated solution outlet
It is exported with a permeate, concentrated solution outlet is connected by pipeline with pressure regulator valve 4, and the liquid outlet of heat exchanger 5 passes through pipeline and material
Tank 1 is connected,
This method is specific as follows:
(1) nucleotide secondary crystallization mother liquor is placed in batch can 1, starts delivery pump 2, nucleotide secondary crystallization mother liquor is led to
It crosses membrane module 3 and is concentrated 5 times, final anti-yield is greater than 99%；The operating pressure of the equipment be 20~28bar, temperature be 23~
30 DEG C, average flux is 25~30LMH；
(2) then the residual liquid being rinsed with water in mold core and pipeline is cleaned under conditions of 30~40 DEG C with cleaning solution
0.4~0.6h can restore mold core flux substantially.
Nucleotide secondary crystallization mother liquor concentrations stablize experiment and have carried out 2 batches in total according to the above method, take respectively appropriate
Nucleotide secondary crystallization mother liquor tested, in 20-28bar, first batch experimental temperature is controlled 25 for operating pressure control
DEG C or so, the control of second lot experimental temperature compares experiment at 30 DEG C or so, and in terms of experimental test data, temperature gets over low yield
Product transmitance is lower, is lower than 0.02g/L in 25 DEG C of experimental waste liquid contents, 30 DEG C of experimental temperature contents are lower than 0.4g/L；To secondary
De- mother liquor can be concentrated 5 times or so, and average operating flux reaches 25-30LM, and the anti-yield of product is greater than 99%.Detailed Experimental data
It see the table below 3 and Fig. 3:
Table 3: experimental data
Analysis of experimental results
In running temperature control in 30 DEG C, operated under conditions of operating pressure 20-28bar, secondary de- mother liquor can
To be concentrated 5-6 times, average flux reaches 25-30LMH；The anti-yield of product yield can achieve 99% or more, experimentation flux
Curvilinear motion meets film core moving law, and relatively low in initial stage feed concentration, flux is larger, opens with concentration flux
Begin to decline.
Those of ordinary skill in the art still are able to it is found that when technical solution of the present invention changes in following ranges
To same as the previously described embodiments or similar technical effect:
A kind of nucleosides acid mother liquor desalination and concentration method, device therefor include passing sequentially through batch can that pipeline is connected, defeated
Pump, membrane module, pressure regulator valve and heat exchanger are sent, wherein the mold core of membrane module is 3B01 nanofiltration membrane, which has a concentrate
Outlet and permeate outlet, concentrated solution outlet is connected by pipeline with pressure regulator valve, the liquid outlet of heat exchanger pass through pipeline and
Batch can is connected,
This method is specific as follows:
(1) nucleosides acid mother liquor is placed in batch can, start delivery pump, by nucleosides acid mother liquor by membrane module be concentrated 2.8~
After 3.3 times, continues continual add into batch can as needed and continue with the isometric water of the amount of the permeate generated immediately
Operation, total amount of water are equal to the 70% of above-mentioned nucleosides acid mother liquor volume, and final Na removal rate is that 71~80%, Cl removal rate is
93.2~93.8%, 0.05g/L is lower than by the content of liquid nucleotide, positive and negative yield is all larger than 99%.；
(2) then the residual liquid being rinsed with water in mold core and pipeline is cleaned under conditions of 30~40 DEG C with cleaning solution
0.4~0.6h can restore mold core flux substantially.
The foregoing is only a preferred embodiment of the present invention, the range that the present invention that therefore, it cannot be limited according to is implemented, i.e.,
Equivalent changes and modifications made in accordance with the scope of the invention and the contents of the specification should still be within the scope of the present invention.
Claims (5)
1. a kind of nucleosides acid mother liquor desalination and concentration method, it is characterised in that: its device therefor includes passing sequentially through pipeline to be connected
Batch can, delivery pump, membrane module, pressure regulator valve and heat exchanger, wherein the mold core of membrane module is 3B01 nanofiltration membrane, which has
One concentrated solution outlet and permeate outlet, concentrated solution outlet are connected by pipeline with pressure regulator valve, and the liquid outlet of heat exchanger is logical
Pipeline is crossed to be connected with batch can,
This method is specific as follows:
(1) nucleosides acid mother liquor is placed in batch can, starts delivery pump, nucleosides acid mother liquor is concentrated 2.5~5 times by membrane module
Afterwards, continue the continual addition water isometric with the amount of the permeate generated immediately into batch can as needed to continue to run,
Total amount of water is equal to the 65~75% of above-mentioned nucleosides acid mother liquor volume, and final positive and negative yield is all larger than 99%；Above equipment
Operating pressure is 20~28bar, and temperature is 20~30 DEG C, and average flux is 12~30LMH；
(2) residual liquid being rinsed with water in mold core and pipeline, then 0.4 is cleaned under conditions of 30~40 DEG C with cleaning solution~
0.6h can restore mold core flux substantially；
Above-mentioned nucleosides acid mother liquor is nucleotide primary crystallization mother liquor or nucleotide secondary crystallization mother liquor.
2. a kind of nucleosides acid mother liquor desalination and concentration method as described in claim 1, it is characterised in that: the operation pressure of the equipment
Power is 20~26bar, and temperature is 20~26 DEG C, and average flux is 12~13.5LMH.
3. a kind of nucleosides acid mother liquor desalination and concentration method as claimed in claim 2, it is characterised in that: the step (1) are as follows: will
Nucleosides acid mother liquor is placed in batch can, starts delivery pump, after nucleosides acid mother liquor is concentrated 2.8~3.3 times by membrane module, continues root
It is continued to run according to the continual addition water isometric with the amount of the permeate generated immediately into batch can of needs, total amount of water
Equal to the 70% of above-mentioned nucleosides acid mother liquor volume, final Na removal rate is that 71~80%, Cl removal rate is 93.2~93.8%, is led to
The content of liquid nucleotide is crossed lower than 0.05g/L, positive and negative yield is all larger than 99%.
4. a kind of nucleosides acid mother liquor desalination and concentration method as described in claim 1, it is characterised in that: the operation pressure of the equipment
Power is 20~28bar, and temperature is 23~30 DEG C, and average flux is 25~30LMH.
5. a kind of nucleosides acid mother liquor desalination and concentration method as claimed in claim 4, it is characterised in that: the step (1) are as follows: will
Nucleosides acid mother liquor is placed in batch can, starts delivery pump, nucleosides acid mother liquor is concentrated 5 times by membrane module, final anti-yield is greater than
99%.
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| CN201610520997.2A CN106188189B (en) | 2016-07-04 | 2016-07-04 | A kind of nucleosides acid mother liquor desalination and concentration method |
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| CN201610520997.2A CN106188189B (en) | 2016-07-04 | 2016-07-04 | A kind of nucleosides acid mother liquor desalination and concentration method |
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| CN106188189A CN106188189A (en) | 2016-12-07 |
| CN106188189B true CN106188189B (en) | 2019-04-16 |
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| CN111704637A (en) * | 2020-06-28 | 2020-09-25 | 南京工业大学 | Method for refining nucleotide by adopting membrane distillation crystallization |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884523A (en) * | 2006-06-13 | 2006-12-27 | 南京工业大学 | Method for separating and preparing 5'-nucleotide using emulated moving bed |
| CN101418327A (en) * | 2008-11-21 | 2009-04-29 | 大连珍奥生物技术股份有限公司 | The new process of production of high purity 5 ' Nucleotide |
| CN103127833A (en) * | 2013-02-05 | 2013-06-05 | 山东兆光色谱分离技术有限公司 | Nanofiltration membrane system applied to fermented liquid purification |
-
2016
- 2016-07-04 CN CN201610520997.2A patent/CN106188189B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1884523A (en) * | 2006-06-13 | 2006-12-27 | 南京工业大学 | Method for separating and preparing 5'-nucleotide using emulated moving bed |
| CN101418327A (en) * | 2008-11-21 | 2009-04-29 | 大连珍奥生物技术股份有限公司 | The new process of production of high purity 5 ' Nucleotide |
| CN103127833A (en) * | 2013-02-05 | 2013-06-05 | 山东兆光色谱分离技术有限公司 | Nanofiltration membrane system applied to fermented liquid purification |
Non-Patent Citations (1)
| Title |
|---|
| 纳滤膜技术在核苷酸浓缩中的应用;姚志春;《甘肃科学学报》;20050630;第17卷(第2期);第64-66页第1-4节 |
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