CN112062796B - Acarbose continuous desalting and neutralizing production method based on continuous ion exchange device - Google Patents
Acarbose continuous desalting and neutralizing production method based on continuous ion exchange device Download PDFInfo
- Publication number
- CN112062796B CN112062796B CN202011194090.4A CN202011194090A CN112062796B CN 112062796 B CN112062796 B CN 112062796B CN 202011194090 A CN202011194090 A CN 202011194090A CN 112062796 B CN112062796 B CN 112062796B
- Authority
- CN
- China
- Prior art keywords
- resin
- station
- area
- continuous
- regeneration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/20—Carbocyclic rings
- C07H15/203—Monocyclic carbocyclic rings other than cyclohexane rings; Bicyclic carbocyclic ring systems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/02—Column or bed processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/60—Cleaning or rinsing ion-exchange beds
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Water Treatment By Electricity Or Magnetism (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention relates to an acarbose continuous desalting and neutralizing production method based on a continuous ion exchange device, wherein acarbose plate frame filtrate passes through the continuous ion exchange device filled with desalting and neutralizing separation resin, and the steps of feeding, washing, reverse regeneration, backwashing, regeneration, flushing and the like which are carried out according to the time lapse in the traditional production are realized in a continuous production method, so that the product is continuously fed and continuously discharged, and the traditional fixed bed technology is completely reformed. In the continuous operation of the continuous ion exchange unit of the present invention, the sequential switching of the various fluid distribution valves, each separation unit will pump in sequence liquids of different media such as: raw materials, water, different chemical reagents, etc. The resin which is already worked enters a regeneration zone along with the rotation of the system, and the separation column can continue to work after the regeneration zone is regenerated and washed.
Description
Technical Field
The invention relates to the technical field of product desalination and neutralization, in particular to a continuous acarbose desalination and neutralization production method based on a continuous ion exchange device.
Background
The filter liquor obtained after filtering the acarbose fermentation liquor by a plate frame is prepared by adding potassium dihydrogen phosphate, sodium dihydrogen phosphate, ferric chloride and calcium chloride which are added in a fermentation way, ions brought by underground water and aluminum sulfate which is added by a flocculating agent into feed liquid, so that the feed liquid contains various metal cations: iron, magnesium, aluminum, calcium, potassium and the like, wherein the plate-frame filtrate needs to be desalted by using cation resin to remove metal ions and inorganic salts in the feed liquid, and then the salt in the feed liquid is neutralized to ph7.5 or below by using anion resin to achieve the aim of removing the salt in the feed liquid.
In the prior art, the aca desalting neutralization section adopts an old fixed bed mode, so that the use link is complicated, the operation is more, the yield is not high, and the production is not facilitated. In order to improve the yield of acarbose and reduce the misoperation of human factors, the invention provides a new process, namely a two-in-one continuous ion-exchange separation process.
Disclosure of Invention
The technical problem to be solved by the invention is to provide an acarbose continuous desalting and neutralizing production method based on a continuous ion exchange device, aiming at the defects of complicated steps, low yield, high cost and the like of the existing acarbose production method, and the invention provides an improved acarbose production method based on an advanced separation method of the continuous ion exchange device so as to achieve the purposes of reducing the production cost, simplifying the production method, shortening the production period and improving the total yield.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a continuous acarbose desalting and neutralizing production method based on a continuous ion exchange device has the key technology that:
the continuous ion exchange device comprises a plurality of separation units and a rotary switching valve, wherein the separation units are arranged around the rotary switching valve in a circumferential manner, the rotary switching valve is provided with stations with the same number as the separation units, each station is provided with a feed inlet and a discharge outlet, the discharge outlets of the rotary switching valve are in butt joint with the feed inlets of the separation units, the feed inlets of the rotary switching valve are in butt joint with the discharge outlets of the separation units, different materials are connected with each separation unit through the rotary switching valve, and the separation units and the rotary switching valve synchronously rotate to change stations;
one part of the plurality of separation units is a positive resin separation unit filled with desalted positive resin, and the other part is a negative resin separation unit filled with negative resin; the positive resin separation unit is used for desalting, and the negative resin separation unit is used for neutralizing;
the production method comprises the following steps:
the positive resin zones being in a cyclic sequence
Backwashing the cation resin: at least 1 station is an anode resin backwashing water area, deionized water is fed from the bottom of the anode resin separation unit and discharged from the top in a bottom-up feeding mode;
cation resin regeneration: more than 2 stations are anode resin acid regeneration zones, the separation units of the anode resin acid regeneration zones are connected in series, HCl solution is introduced into the inlet of the first station of the zones, and the HCl solution is discharged from the outlet of the last station;
acid washing of cation resin: more than 2 stations are positive resin acid washing areas, the separation units of the positive resin acid washing areas are connected in series, deionized water is introduced from the first station of the positive resin acid washing areas, and the deionized water is discharged from the last station of the positive resin acid washing areas;
desalting the cation resin: the plurality of stations are cation resin desalting regions, the separating units of the regions are connected in series, acarbose plate frame filtrate enters from the first station of the regions in a forward mode, is desalted by the plurality of separating units, and the feed liquid is discharged from the last station to a anion resin neutralizing region for neutralization;
cation resin washing: at least 1 station is a cation resin washing area, deionized water adopts a positive feeding mode, and outlet shower water is connected in series with an inlet of a first station of a cation resin desalting area;
and (3) reverse regeneration of the cation resin: at least 1 station is a cation resin reverse regeneration zone, NaOH solution is fully contacted with the cation resin by adopting a reverse feeding mode from bottom to top, and the NaOH solution at an outlet is discharged;
the negative resin zone being in a cyclic sequence
And (3) backwashing of anion resin: at least 1 station is an anion resin backwashing water area, deionized water is fed from the bottom of the anion resin separation unit in a bottom-up feeding mode, and is discharged from the top; .
Regeneration of the anion resin: more than 2 stations are anion resin alkali regeneration zones, the separation units of the anion resin alkali regeneration zones are connected in series, NaOH solution is introduced into the first station of the zone, and the last station is discharged from an outlet;
alkali washing of anion resin: more than 2 stations are anion resin alkali washing areas, the separation units of the anion resin alkali washing areas are connected in series, deionized water is introduced from the first station of the areas, and the deionized water is discharged from the last station;
and (3) anion resin neutralization: the plurality of stations are negative resin neutralization areas, the area separation units are connected in series and are connected with the discharge hole of the positive resin desalination area in series, the feed liquid discharged from the positive resin desalination area enters the negative resin neutralization area from the first station of the area in a reverse-feeding mode, and the feed liquid neutralized by the negative resin is discharged from the last station of the area, so that the product obtained by the production method is obtained;
washing the material with anion resin: at least 1 station is a negative resin washing area, deionized water enters in a positive feeding mode, and outlet shower water is connected in series with an inlet of a first station in a negative resin neutralization area;
reverse regeneration of the negative resin: at least 1 station is a negative resin reverse regeneration zone, HCl solution is fully contacted with the negative resin by adopting a reverse feeding mode from bottom to top, and HCl solution at an outlet is discharged.
All the cation resin separation units are arranged around a circumference and sequentially divided into an cation resin backwashing area, an cation resin regeneration area, an cation resin acid washing area, an cation resin desalting area, an cation resin material washing area and an cation resin reverse regeneration area; in the same way, all the anion resin separation units are sequentially divided into an anion resin backwashing area, an anion resin regeneration area, an anion resin acid washing area, an anion resin neutralization area, an anion resin material washing area and an anion resin reverse regeneration area.
All the zones of the cation resin separation unit are connected end to end, rotate continuously, switch stations, further switch materials, realize desalination and regeneration and work continuously; similarly, all the areas of the anion resin separation unit are connected end to end, rotate continuously, switch stations, further switch materials, realize neutralization and regeneration, and work continuously.
The number of the separation units contained in each zone depends on the process requirements, and the index of the final product at the outlet of the anionic resin neutralization zone reaches the process requirements.
As a further improvement of the invention, the conductance of the product material at the outlet of the anion resin neutralization zone is below 300us/cm, and the pH value is 5.5-7.5.
As a further improvement of the invention, in the cation resin acid regeneration zone, the mass concentration of the outlet acid is not lower than 2%; and in the negative resin alkali regeneration zone, the mass concentration of the outlet alkali is not lower than 2%.
As a further improvement of the invention, the electric conductivity of outlet water of the acid washing area of the cation resin and the alkali washing area of the anion resin is lower than 100 mu s/cm.
As a further improvement of the invention, the mass concentration of HCl solution introduced into the positive resin regeneration zone and the negative resin reverse regeneration zone is 4-8%; the mass concentration of NaOH solution introduced into the positive resin reverse regeneration zone and the negative resin regeneration zone is 4-8%.
As a further improvement of the invention, the conductivity of the outlet water when the sample is taken before the last separation unit in the cation resin acid washing area rotates is less than 100 mus/cm.
As a further improvement of the invention, the outlet water conductivity of the last separation unit of the anion resin alkali washing area is sampled before rotation selection, and is lower than 100 mus/cm.
As a further improvement of the invention, the outlet of the last station of the cation resin acid washing area is connected with the first station of the cation resin acid regeneration area in series.
As a further improvement of the invention, the outlet of the last station of the anion resin alkali washing area is connected with the first station of the anion resin alkali regeneration area in series.
As a further improvement of the invention, one half of the plurality of separation units is a male resin separation unit, the other half of the plurality of separation units is a female resin separation unit, and the male resin separation unit and the female resin separation unit are vertically and fixedly connected to form a two-in-one integral structure.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
1. the process is integrated, the production efficiency is improved, and the production period is shortened.
2. And errors caused by manual operation are reduced.
3. Continuously running and continuously discharging.
4. The two-in-one continuous ion exchange technology has the following advantages:
1) due to continuous operation, the product components and concentration are kept stable, and the matching of a downstream working section is facilitated.
2) Because of improving production efficiency, the resin column, the storage tank and the matching scale are very small, the equipment is compact, the resin column, the storage tank and the matching scale are easy to install at any position, the resin column is easy to match with the old production process and the equipment, and the occupied area is only about one third of the same scale.
3) The rotation speed can be automatically adjusted according to the requirements of the production process along with the change of the mass and the flow rate of the inflow fluid, thereby ensuring the operation under the economically optimal state.
4) The acid and alkali consumption is reduced, the wastewater discharge is reduced, and the subsequent environmental protection pressure is relieved.
5) Due to the adoption of a plurality of separation units, the production method flow can be flexibly changed.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic diagram of the rotary switching valve after the station functional area division is expanded.
FIG. 2 is a schematic diagram of the material process of the present invention.
In fig. 1 and 2:
100-rotating switching valve;
200-separation unit.
Detailed Description
For purposes of clarity and a complete description of the present invention, and the like, in conjunction with the detailed description, it is to be understood that the terms "central," "vertical," "lateral," "up," "down," "front," "back," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings for convenience in describing and simplifying the present invention, but do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be considered as limiting the present invention.
A continuous acarbose desalting and neutralizing production method based on a continuous ion exchange device adopts a two-in-one continuous ion exchange device filled with desalting cation resin and neutralizing anion resin to realize the desalting and neutralizing of acarbose through the two-in-one continuous ion exchange.
The two-in-one continuous ion exchange system is internally provided with 30 separation units and a rotary switching valve, 15 separation units are filled with desalting cation resin, and 15 separation units are filled with neutralizing anion resin, wherein one cation resin separation unit and one anion resin separation unit are vertically and fixedly connected to form a two-in-one integral structure, so that the occupied area of equipment used in the whole process method is reduced. The separation unit is a resin column.
The rotary switching valve is provided with 30 stations 1# -30#, each station is provided with a feed inlet and a discharge outlet, the discharge outlet is in butt joint with the feed inlet of the separation unit, the feed inlet is in butt joint with the discharge outlet of the separation unit, and different materials are connected with each separation unit through the rotary switching valve.
The 30 separation units are arranged around the rotary switching valve in a circumferential mode, the 30 separation units rotate one station every certain time, and the valve bodies of the rotary switching valve rotate synchronously with the rotary switching valve, so that all the separation units synchronously change stations.
As shown in fig. 1, on the rotary switching valve, stations 1#, 3#, 5#, 7#, 9#, 11#, 13#, 15#, 17#, 19#, 21#, 23#, 25#, 27#, and 29# correspond to the separation units filled with the male resin; the 2#, 4#, 6#, 8#, 10#, 12#, 14#, 16#, 18#, 20#, 22#, 24#, 26#, 28# and 30# stations correspond to the separation units filled with the female resin.
As shown in FIG. 2, when each of the female resin separation unit and the male resin separation unit rotates to the station No. 1-30, the corresponding material is connected with other separation units through a rotary switching valve. In fig. 2, the number 1# … … 30# marked on the separating unit is the station number of the rotary switching valve corresponding to the separating unit at the position, the station on the rotary switching valve is relatively fixed, and the corresponding separating unit rotates in the device to switch the station. The continuous ion exchange device is provided with a bottom rotating disk, all the separation units are fixedly arranged on the rotating disk, a valve body of the rotary switching valve is fixed right above the center of the rotary switching disk, and a rotating part of the rotary switching valve synchronously rotates along with the rotating disk. And when the rotating disc rotates once, all the separation units sequentially enter the next adjacent station, and then stay for a certain time to process the materials, wherein the stay time interval is determined according to the process requirement, for example, a certain index of the materials at the material outlet of a specific station, if the process requirement is met, the separation units rotate to enter the next station, and if the process requirement is not met, the material processing is continued.
In this example, the pH of the acarbose plate-frame filtrate was 3.5-4.6, the conductance was 7000-. The resin filling amount of each separation unit was 200L; the feed rate of the acarbose feed liquid was 3 t/h.
Based on the two-in-one continuous ion exchange system, the production method for continuously desalting and neutralizing acarbose comprises the following steps:
positive resin zone
Backwashing the cation resin: the No. 1 station is a positive resin backwashing water area, deionized water is fed from the bottom to the top of the positive resin separation unit in a feeding mode from bottom to top, the top of the positive resin separation unit is discharged, and discharged water is directly discharged into wastewater. The method is mainly used for flushing pollutants generated by reverse regeneration, and on the other hand, the loose resin enables the resin not to influence the adsorption effect easily due to hardening.
Cation resin regeneration: the 25#, 27# and 29# stations are cation resin acid regeneration zones, separation units of the cation resin acid regeneration zones are connected in series, HCl solution with the mass concentration of 4% -8% is introduced into the 25# station, and the HCl solution is discharged from an outlet of the 29# station and then discharged into wastewater; the cation resin acid regeneration zone adopts three columns connected in series (because the work station is in rotary switching, a gradient regeneration mode is formed), thereby achieving the purposes of reusing acid and saving materials; to ensure complete regeneration, the separation unit at station # 29 of the cation resin acid regeneration zone was sampled prior to rotation to ensure that the outlet acid concentration was not less than 2%. The concentration of the HCl solution is preferably 6%.
Acid washing of cation resin: the 21# and 23# stations are positive resin acid washing areas, the separation units of the positive resin acid washing areas are connected in series, deionized water is introduced from the 21# station, the 23# station is discharged and then connected in series with the 25# station, and the deionized water is fed in a forward mode. The acid washing area of the cation resin adopts a gradient water washing mode (namely, stations are connected in series and are rotationally switched), so that the water consumption is saved. To ensure clean water washing, the last separation unit in the acid washing area of the cation resin is sampled before rotation, and the electric conductivity of outlet water is lower than 100 mus/cm.
Desalting the cation resin: the separation units filled with the positive resin and corresponding to the stations 7#, 9#, 11#, 13#, 15#, 17# and 19# are positive resin desalting areas, the seven separation units are connected in series, acarbose plate frame filtrate enters from the station 7# in a positive mode and is desalted by the seven separation units filled with the positive resin, and feed liquid is discharged from the station 19# to a negative resin neutralizing area for neutralization. The separation unit in the cation resin desalting area is easy to cause empty columns due to bubbles generated by feed liquid, so that preferably, acarbose plate frame filtrate is firstly pumped into a transfer tank and then is pumped into a 7# station from the transfer tank. Set up the convenient exhaust of material transfer tank on the one hand, on the other hand positive resin ejection of compact feed liquid misce bene guarantees ejection of compact product quality.
Cation resin washing: the No. 5 station is a positive resin washing area, deionized water adopts a positive feeding mode, and outlet shower water is connected with an inlet of the No. 7 station in series; the washing material has certain complementary effect on the purity and the yield of the product, and particularly can ensure the yield of the product.
And (3) reverse regeneration of the cation resin: the No. 3 station is a positive resin reverse regeneration area, the NaOH solution adopts a reverse feeding mode from bottom to top to ensure that the alkali liquor with the mass concentration of 4-8% is fully contacted with the positive resin, so that impurities such as protein and the like polluting the resin are fully reacted with the alkali, and then pollutants are converged to the upper part of a resin column along the flowing direction of water flow, and are conveniently discharged during backflushing; and discharging the NaOH solution at an outlet to waste water. The mass concentration of the NaOH solution is preferably 6%.
Negative resin region
And (3) backwashing of anion resin: the No. 2 station is an anion resin backwashing water area, deionized water is fed from the bottom of the anion resin separation unit in a feeding mode from bottom to top, and is discharged to wastewater from the top. The method is mainly used for flushing pollutants generated by reverse regeneration, and on the other hand, the loose resin enables the resin not to influence the adsorption effect easily due to hardening.
Regeneration of the anion resin: the 26#, 28# and 30# stations are negative resin alkali regeneration areas, the separation units of the negative resin alkali regeneration areas are connected in series, NaOH solution with the mass concentration of 4% -8% is introduced into the 26# station, and the NaOH solution is discharged from a 30# outlet; a gradient regeneration mode is adopted to save the consumption of alkali; in order to ensure that the regeneration of the negative resin is complete, the last separation unit in the alkali regeneration area of the negative resin samples before rotation, and the alkali concentration at the discharge hole of the 30# station is ensured to be not lower than 2%. The mass concentration of the NaOH solution is preferably 6%.
Alkali washing of anion resin: the 20#, 22#, and 24# stations are anion resin alkali washing areas, the separation units of the anion resin alkali washing areas are connected in series, and deionized water enters from the 20# station in a positive feeding mode, is discharged from the 24# station and then is connected in series with the 26# station. And a series mode is adopted, so that the flushing efficiency is improved, and in order to ensure that the water is washed cleanly, the last separation unit in the anion resin alkali washing area is sampled before selection, and the water conductivity at the outlet is lower than 100 mu s/cm.
And (3) anion resin neutralization: the 6#, 8#, 10#, 12#, 14#, 16# and 18# stations are female resin neutralization areas, the six separation units are connected in series and are connected in series with the discharge hole of the male resin desalting area, the feed liquid discharged from the 19# station enters the female resin neutralization area from the 8# station in a counter-feeding mode, and the feed liquid neutralized by female resin is discharged from the 18# station, so that the product obtained by the process method is obtained.
Washing the material with anion resin: the No. 6 station is a negative resin washing area, deionized water enters in a positive feeding mode, and outlet shower water is connected with an inlet of the No. 8 station in series; the washing material has certain complementary effect on the purity and the yield of the product, and particularly can ensure the yield of the product.
Reverse regeneration of the negative resin: the No. 4 station is a negative resin reverse regeneration zone, HCl solution adopts a reverse feeding mode from bottom to top to ensure that hydrochloric acid solution with the mass concentration of 4-8% is fully contacted with the negative resin, and HCl solution at an outlet is discharged to wastewater. Because a large amount of carbonate exists in the anion resin pollution, a large amount of bubbles are generated when the anion resin is reversely regenerated by using hydrochloric acid, and the pollutants and the hydrochloric acid can fully react while the bubbles are conveniently removed by a feeding mode from bottom to top, so that the resin pollution degree is reduced. The HCl solution is preferably at a concentration of 6%.
Wherein, the feeding speed of the deionized water in the positive resin backwashing water zone and the negative resin backwashing water zone is 4 t/h.
Wherein, the feeding speed of the deionized water in the positive resin washing area and the negative resin washing area is 2 t/h.
Wherein, the feeding speed of hydrochloric acid with the mass concentration of 6 percent in the cation resin acid regeneration zone is 1.8t/h for regenerating the cation resin.
Wherein, in the anion resin alkali regeneration zone, the feeding speed of NaOH solution with the mass concentration of 6 percent is 2t/h for regenerating anion resin.
Wherein, in the cation resin acid washing area, the feeding speed of the deionized water is 4t/h, and the cation resin acid washing area is used for washing the cation resin.
Wherein, in the anion resin alkali washing area, the feeding speed of the deionized water is 4.2t/h, and the anion resin alkali washing area is used for washing anion resin.
Wherein, the cation resin reverse regeneration zone has a NaOH solution feeding speed of 2t/h with a mass concentration of 6 percent and is used for cleaning impurities such as protein and the like in the cation resin.
Wherein, the feeding speed of the hydrochloric acid with the mass concentration of 6% in the negative resin reverse regeneration zone is 2t/h, and the negative resin reverse regeneration zone is used for cleaning the pollution of inorganic salt and the like of the negative resin.
The feed rate of the above-mentioned materials can also be adjusted within a reasonable range according to the process requirements, subject to the preset index of the final acarbose product. For example, the high quality of acarbose plate frame filtrate is low, the number of separation units and the resin filling amount thereof will affect subsequent feeding indexes (including concentration, speed, residence time, etc.), and those skilled in the art can understand that, on the premise of meeting the requirements of the process indexes of export products, the conditions of saving space, reducing production cost, improving production efficiency, guaranteeing product quality, etc. are the final targets of adjusting various process parameters. However, the above production method is a preferred technical solution in the quality of acarbose plate-frame filtrate provided in this example.
In the present embodiment, when describing the steps of the production method, the positive resin region, the negative resin region, and each of the different functional regions are arranged in sequence, but in the actual production process, after the device is operated, each region performs corresponding work at the same time. However, when the equipment is initially started, the aca liquid can be introduced only after backwashing, regeneration and the like.
The invention adopts the advanced separation method of the continuous ion exchange device to replace a fixed bed separation column in the traditional method. The design improvement production method comprises the following processes:
acarbose plate-frame mixed liquor-transfer tank-continuous ion exchange device-acarbose feed liquid-downstream working section.
The method is characterized in that acarbose mixed liquor passes through a continuous ion exchange device filled with desalting neutralizing separation resin, in a continuous ion exchange unit, according to different adsorption forces of the resin on acarbose and inorganic salt, the effluent is acarbose, the worked resin enters a regeneration zone along with the rotation of the system, and after regeneration and leaching are carried out in the regeneration zone, a separation column can continue to work.
The continuous ion exchange device technology used by the production method provided by the invention realizes the steps of feeding, washing, reverse regeneration, backwashing, regeneration, flushing and the like according to the time lapse in the traditional production in a continuous production method, continuously feeds materials and continuously discharges products, and completely renovates the traditional fixed bed technology. In the continuous operation of the continuous ion exchange unit of the present invention, the sequential switching of the various fluid distribution valves, each separation unit will pump in sequence liquids of different media such as: raw materials, water, different chemical reagents, etc.
The continuous ion exchange adopts a yin-yang integrated design acarbon frame filtrate continuous ion exchange treatment system, the feed liquid is acarbon frame filtrate pH3.5-4.6, the electric conductivity 7000-. The transmittance of the filter liquor of the acanthus frame is 40-60%; on the premise that the system operates with a feeding amount of 80-100ml/min, the yin-yang integrated design ensures that the positive calculation yield is more than 92%, the negative calculation yield is more than 95%, the mixed discharging conductance of the product is less than 300us/cm, and the pH is less than 7.5; compared with the prior fixed bed, the resin consumption can be saved by more than 90 percent, the unit consumption can be saved by 24 percent according to the unit feeding amount, the unit consumption of acid can be saved by 56 percent, the unit consumption of alkali can be saved by 48 percent, and the wastewater discharge can be reduced by nearly 40 percent.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A continuous acarbose desalting and neutralizing production method based on a continuous ion exchange device is characterized in that:
the continuous ion exchange device comprises a plurality of separation units and a rotary switching valve, wherein the separation units are arranged around the rotary switching valve in a circumferential manner, the rotary switching valve is provided with stations with the same number as the separation units, each station is provided with a feed inlet and a discharge outlet, the discharge outlets of the rotary switching valve are in butt joint with the feed inlets of the separation units, the feed inlets of the rotary switching valve are in butt joint with the discharge outlets of the separation units, different materials are connected with each separation unit through the rotary switching valve, and the separation units and the rotary switching valve synchronously rotate to change stations;
one part of the plurality of separation units is a positive resin separation unit filled with desalted positive resin, and the other part is a negative resin separation unit filled with negative resin;
in the plurality of separation units, one half of the separation units are male resin separation units, the other half of the separation units are female resin separation units, and the male resin separation units and the female resin separation units are vertically and fixedly connected to form a two-in-one integral structure;
the production method comprises the following steps:
the positive resin zones being in a cyclic sequence
Backwashing the cation resin: at least 1 station is an anode resin backwashing water area, deionized water is fed from the bottom of the anode resin separation unit and discharged from the top in a bottom-up feeding mode;
cation resin regeneration: more than 2 stations are anode resin acid regeneration zones, the separation units of the anode resin acid regeneration zones are connected in series, HCl solution is introduced into the inlet of the first station of the zones, and the HCl solution is discharged from the outlet of the last station;
acid washing of cation resin: more than 2 stations are positive resin acid washing areas, the separation units of the positive resin acid washing areas are connected in series, deionized water is introduced from the first station of the positive resin acid washing areas, and the deionized water is discharged from the last station of the positive resin acid washing areas;
desalting the cation resin: the plurality of stations are cation resin desalting regions, the separating units of the regions are connected in series, acarbose plate frame filtrate enters from the first station of the regions in a forward mode, is desalted by the plurality of separating units, and the feed liquid is discharged from the last station to a anion resin neutralizing region for neutralization;
cation resin washing: at least 1 station is a cation resin washing area, deionized water adopts a positive feeding mode, and outlet shower water is connected in series with an inlet of a first station of a cation resin desalting area;
and (3) reverse regeneration of the cation resin: at least 1 station is a cation resin reverse regeneration zone, NaOH solution is fully contacted with the cation resin by adopting a reverse feeding mode from bottom to top, and the NaOH solution at an outlet is discharged;
the negative resin zone being in a cyclic sequence
And (3) backwashing of anion resin: at least 1 station is an anion resin backwashing water area, deionized water is fed from the bottom of the anion resin separation unit in a bottom-up feeding mode, and is discharged from the top;
regeneration of the anion resin: more than 2 stations are anion resin alkali regeneration zones, the separation units of the anion resin alkali regeneration zones are connected in series, NaOH solution is introduced into the first station of the zone, and the last station is discharged from an outlet;
alkali washing of anion resin: more than 2 stations are anion resin alkali washing areas, the separation units of the anion resin alkali washing areas are connected in series, deionized water is introduced from the first station of the areas, and the deionized water is discharged from the last station;
and (3) anion resin neutralization: the plurality of stations are negative resin neutralization areas, the area separation units are connected in series and are connected with the discharge hole of the positive resin desalination area in series, the feed liquid discharged from the positive resin desalination area enters the negative resin neutralization area from the first station of the area in a reverse-feeding mode, and the feed liquid neutralized by the negative resin is discharged from the last station of the area, so that the product obtained by the production method is obtained;
washing the material with anion resin: at least 1 station is a negative resin washing area, deionized water enters in a positive feeding mode, and outlet shower water is connected in series with an inlet of a first station in a negative resin neutralization area;
reverse regeneration of the negative resin: at least 1 station is a negative resin reverse regeneration zone, HCl solution is fully contacted with the negative resin in a reverse feeding mode from bottom to top, and HCl solution at an outlet is discharged;
the conductance of the product material at the outlet of the anion resin neutralization area is below 300us/cm, and the pH value is 5.5-7.5.
2. The continuous acarbose desalting and neutralizing production method based on the continuous ion exchange device according to claim 1, characterized in that: in the cation resin acid regeneration zone, the mass concentration of outlet acid is not lower than 2%; and in the negative resin alkali regeneration zone, the mass concentration of the outlet alkali is not lower than 2%.
3. The continuous acarbose desalting and neutralizing production method based on the continuous ion exchange device according to claim 1, characterized in that: the electric conductivity of outlet water of the acid washing area of the cation resin and the alkali washing area of the anion resin is lower than 100 mu s/cm.
4. The continuous acarbose desalting and neutralizing production method based on the continuous ion exchange device according to claim 1, characterized in that: the mass concentration of HCl solution introduced into the positive resin regeneration zone and the negative resin reverse regeneration zone is 4-8%; the mass concentration of NaOH solution introduced into the positive resin reverse regeneration zone and the negative resin regeneration zone is 4-8%.
5. The continuous acarbose desalting and neutralizing production method based on the continuous ion exchange device according to claim 1, characterized in that: sampling before the last separation unit in the cation resin acid washing area rotates, wherein the electric conductivity of outlet water is lower than 100 mu s/cm.
6. The continuous acarbose desalting and neutralizing production method based on the continuous ion exchange device according to claim 1, characterized in that: sampling before the last separation unit in the anion resin alkali washing area selects and rotates, wherein the water conductivity at the outlet is lower than 100 mu s/cm.
7. The continuous acarbose desalting and neutralizing production method based on the continuous ion exchange device according to claim 1, characterized in that: the outlet of the last station of the cation resin acid washing area is connected with the first station of the cation resin acid regeneration area in series.
8. The continuous acarbose desalting and neutralizing production method based on the continuous ion exchange device according to claim 1, characterized in that: the outlet of the last station of the anion resin alkali washing area is connected with the first station of the anion resin alkali regeneration area in series.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011194090.4A CN112062796B (en) | 2020-10-30 | 2020-10-30 | Acarbose continuous desalting and neutralizing production method based on continuous ion exchange device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011194090.4A CN112062796B (en) | 2020-10-30 | 2020-10-30 | Acarbose continuous desalting and neutralizing production method based on continuous ion exchange device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112062796A CN112062796A (en) | 2020-12-11 |
| CN112062796B true CN112062796B (en) | 2022-02-22 |
Family
ID=73655796
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011194090.4A Active CN112062796B (en) | 2020-10-30 | 2020-10-30 | Acarbose continuous desalting and neutralizing production method based on continuous ion exchange device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112062796B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112895544A (en) * | 2021-01-16 | 2021-06-04 | 吴飞飞 | Stamping die forming method for printing rubber roller |
| CN113336803B (en) * | 2021-06-03 | 2023-11-21 | 同舟纵横（厦门）流体技术有限公司 | Method for removing mono-disaccharide from acarbose and acarbose purification method |
| CN114606348A (en) * | 2022-03-10 | 2022-06-10 | 欧尚元(天津)有限公司 | Sucrose decoloring method and system |
| CN115057901A (en) * | 2022-07-12 | 2022-09-16 | 赛普特环保技术(厦门)有限公司 | Nucleoside purification system and purification process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003014135A1 (en) * | 2001-08-07 | 2003-02-20 | Biogal Gyogyszergyar Rt | Method for purification of acarbose |
| CN1414003A (en) * | 2002-07-31 | 2003-04-30 | 浙江德清东立生物发展有限公司 | Method for preparing high-purity acarbose |
| CN102030786A (en) * | 2010-11-12 | 2011-04-27 | 丽珠集团新北江制药股份有限公司 | Preparation method of acarbose |
| CN109225355A (en) * | 2018-11-13 | 2019-01-18 | 赛普特环保技术(厦门)有限公司 | A kind of continuous ionic exchange process removing inorganic salts and used system |
| CN111269276A (en) * | 2020-03-13 | 2020-06-12 | 厦门世达膜科技有限公司 | Production method for separating acarbose and impurities |
| CN213222209U (en) * | 2020-09-18 | 2021-05-18 | 石药集团圣雪葡萄糖有限责任公司 | Rotary continuous ion exchange device for acarbose desalination |
-
2020
- 2020-10-30 CN CN202011194090.4A patent/CN112062796B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003014135A1 (en) * | 2001-08-07 | 2003-02-20 | Biogal Gyogyszergyar Rt | Method for purification of acarbose |
| CN1414003A (en) * | 2002-07-31 | 2003-04-30 | 浙江德清东立生物发展有限公司 | Method for preparing high-purity acarbose |
| CN102030786A (en) * | 2010-11-12 | 2011-04-27 | 丽珠集团新北江制药股份有限公司 | Preparation method of acarbose |
| CN109225355A (en) * | 2018-11-13 | 2019-01-18 | 赛普特环保技术(厦门)有限公司 | A kind of continuous ionic exchange process removing inorganic salts and used system |
| CN111269276A (en) * | 2020-03-13 | 2020-06-12 | 厦门世达膜科技有限公司 | Production method for separating acarbose and impurities |
| CN213222209U (en) * | 2020-09-18 | 2021-05-18 | 石药集团圣雪葡萄糖有限责任公司 | Rotary continuous ion exchange device for acarbose desalination |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112062796A (en) | 2020-12-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112062796B (en) | Acarbose continuous desalting and neutralizing production method based on continuous ion exchange device | |
| CN100581640C (en) | Electro-deionization method and device for synchronously concentrating and purifying heavy metal wastewater | |
| CN100482594C (en) | Electrodeionization water-purifying device and method for recovering cation and anion without scaling | |
| CN103060834A (en) | Technological process for electrolyzing sodium sulfate | |
| LU505290B1 (en) | Method for purifying L-lactic acid | |
| CN211913799U (en) | Ion exchange regeneration system | |
| CN201842708U (en) | Purifying device for online separation of metal salt and free acid in pickling solution | |
| CN113527085A (en) | Production method for purifying lactic acid from lactic acid fermentation liquor | |
| CN217628184U (en) | Nucleoside purification system | |
| CN101708908A (en) | Novel method for treating electroplating chromium-containing wastewater and recovering metal ions | |
| CN213222209U (en) | Rotary continuous ion exchange device for acarbose desalination | |
| CN211585316U (en) | System for continuously removing anions in 3-hydroxy-1, 3, 5-pentanedioic acid | |
| CN113336803B (en) | Method for removing mono-disaccharide from acarbose and acarbose purification method | |
| CN202881038U (en) | Electroplating waste water separation and recycling treatment apparatus | |
| CN215559204U (en) | Special film module ware | |
| CN217568776U (en) | Mixed bed device capable of recycling regenerated wastewater | |
| CN109336284A (en) | A kind of waste electroplating liquor containing chromium advanced treating and recoverying and utilizing method | |
| CN202164187U (en) | Device for recycling electroplating rinsing water | |
| CN212640167U (en) | Membrane diffusion coagulation pretreatment system | |
| CN209791565U (en) | Freely-switched regenerated anion exchanger | |
| CN1031527A (en) | From isoelectric point crystallizing mother liquor, reclaim the novel process of L-glutamic acid | |
| CN217627934U (en) | Integrated continuous ion exchange desalination system | |
| CN217555960U (en) | Electroplating wastewater treatment system for printing mold | |
| CN216987715U (en) | Trehalose decoloration purification system | |
| CN218435399U (en) | Chemical nickel waste water resourceful treatment device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |