CN104829446A - Method for extracting sodium gluconate without generating mother liquor - Google Patents
Method for extracting sodium gluconate without generating mother liquor Download PDFInfo
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- CN104829446A CN104829446A CN201510182799.5A CN201510182799A CN104829446A CN 104829446 A CN104829446 A CN 104829446A CN 201510182799 A CN201510182799 A CN 201510182799A CN 104829446 A CN104829446 A CN 104829446A
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- sodium gluconate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention relates to a method for extracting sodium gluconate without generating any mother liquor, which comprises the concrete steps of (1) modulating the solution concentration; (2) inoculating; (3) crystallizing and drying; (4) and collecting finished products. According to the technical scheme of the invention, through controlling the proportion of the sodium gluconate solution to the sodium gluconate seed crystal, a normal-pressure high-temperature super-saturated solution balanced in concentration distribution can be obtained. Meanwhile, through controlling the granularity, the super-saturation degree, the homogeneous feedstock, the orifice size of a two-fluid nozzle, the flow rate and the jet velocity of a drying air flow, and the flow rate and the jet velocity of the super-saturated solution, the sodium gluconate, which enters a drying chamber, can quickly adhere onto the seed crystal to be coagulated. Therefore, sodium gluconate crystals of uniform granularity and plump particles can be formed. The above technical scheme is applicable to the sodium gluconate solution prepared through various sodium gluconate-based production methods, such as two-enzyme method, metal catalytic method, fermentation method and the like. The sodium gluconate can be extracted through one shot without generating any mother liquor. Meanwhile, the de-coloration cost is saved or the de-coloration cost is significantly reduced.
Description
Technical field
The present invention relates to a kind of extracting method not generating the Sunmorl N 60S of mother liquor, be specifically related to extract Sunmorl N 60S to the sodium gluconate solution produced by double-enzyme method or metal catalysed processes or fermentation method etc. and do not generate the method for mother liquor, belong to Sunmorl N 60S manufacture field.
Background technology
Sunmorl N 60S is a kind of organic acid salt, of many uses, highly effective chelating agent can be used as in building, textile printing and dyeing and the industry such as metal finishing and water treatment, steel surface clean-out system, glass cleaner, electroplating industry alumina are painted, can be used as high-efficient retarder, high efficiency water reducing agent etc. at Concrete Industry.Sunmorl N 60S has excellent corrosion-mitigation scale-inhibition effect, is widely used in water quality stabilizer, such as, as industrial circulating cooling water system, low pressure boiler, cooling water of internal combustion engine system etc.Sunmorl N 60S can also regulate acid base equilibrium in human body, to recover neural normal effect, in medicine and foodstuff additive etc., also has extensive use.
The production method of existing Sunmorl N 60S is various, common are metal catalytic oxidation method, fermentation method, double-enzyme method etc., and the sodium gluconate solution color and luster that these methods are produced is low, impurity is few, and simple filtration can be suitable for extracting.But in prior art, the production of Sunmorl N 60S with extract be refining filtering after again by repeatedly evaporative crystallization repeatedly centrifugation extract the dry-matter obtaining Sunmorl N 60S.This leaching process is loaded down with trivial details consuming time, more than time to generate a large amount of mother liquor and be difficult to process.These mother liquors are through repeatedly enrichment, and not only color is dark, residual sugar content increases, glucose sodium saccharate content is also limited.Chinese patent CN103923953A discloses a kind of by the solidified method of gluconic acid mother liquid of sodium of fermentative Production, its treating processes is still loaded down with trivial details, handling object and gluconic acid mother liquid of sodium need pre-treatment not only to need the flame filter press that more use floor space is large, also must at substantial gac auxiliary agent.In this kind of mother liquor, residual sugar is up to 20%-30%, the polysaccharide such as spray-dired disaccharides are difficult in a large number except containing containing toward contact except monose, especially easily molten under polysaccharide hot conditions and snearing wall is difficult to dry, and the easily spray-dired tower body passage of blocking or outlet, easy initiating failure even accident, and material is selected improper for control, the product sugar degree high purity produced is not enough.According to said method produce gluconic acid sodium salt and also fundamentally do not change the long flow path of Sunmorl N 60S leaching process, loaded down with trivial details present situation consuming time, repeatedly generation mother liquor or waste liquor, and auxiliary agent consumption is many, pre-treatment burden is heavy, product purity is low.
Therefore, in prior art Sunmorl N 60S extract process loaded down with trivial details consuming time, generate a large amount of mother liquor, constrain the extraction of Sunmorl N 60S.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of extracting method not generating the Sunmorl N 60S of mother liquor, solve loaded down with trivial details consuming time, the problem that generates a large amount of mother liquor of process that existing Sunmorl N 60S extracts.Technical scheme of the present invention is as follows:
Do not generate an extracting method for the Sunmorl N 60S of mother liquor, concrete steps are as follows:
(1) strength of solution is modulated
Evaporated by sodium gluconate solution after filtering and impurity removing, the mass volume ratio to dry-matter is 48-80%, and be then stored in and adjust brilliant tank, temperature is 62-90 DEG C, and constantly stirs; Preferably, the mass volume ratio of dry-matter is 50%-65%, is stored in and adjusts the temperature in brilliant tank to be 85 DEG C.
(2) inoculate
Sunmorl N 60S crystal seed is inoculated in the solution of step (1) gained, inoculum size is the mass volume ratio of Sunmorl N 60S crystal seed and solution is 5-40%, stir after inoculation, rotating speed is 300-4000rpm/min, and temperature is 62-90 DEG C, and the time is 1-5min, mix, form the constant-pressure and high-temperature supersaturated solution of concentration distribution equilibrium, get supersaturated solution and leave standstill observation, carry out crystallizing and drying when the volume of crystal accounts for 20-30%; In 100ml graduated cylinder, leaving standstill observation in 40 seconds as got supersaturated solution, carrying out crystallizing and drying when the volume of crystal accounts for 20-30%;
Preferably, the Sunmorl N 60S crystal seed inoculated requires full grains, epigranular, and Sunmorl N 60S crystal seed crosses 100-500 mesh sieve; Inoculum size is 15-35%; Rotating speed is 1000-1200rmp/min; Crystal crystallite can be prevented to be destroyed, to prevent crystal from gathering condensation in the generation of inoculation link, then can prevent the blocking of nozzle in subsequent step.Preferred, before inoculation, rear temperature all remains on 85 DEG C ± 0.5 DEG C with inoculation.
(3) crystallizing and drying
Spraying dry is carried out, i.e. crystallizing and drying in the kiln supersaturated solution that step (2) obtains being pumped into the spray-drier with Homogenizing pump homogenous charge.
Enable the spray-drier with Homogenizing pump homogenous charge: open Homogenizing pump, spray-drier, induced draft fan and multi-cyclone, the supersaturated solution that step (2) obtains is pumped into rapidly kiln and carries out spraying dry.Homogenizing pump charging can avoid material to block, and make material continuation in fill process keep fully dispersion with even, this spray-drier can be buied in market.
Further, the described nozzle with the spray atomization system of the spray-drier of Homogenizing pump homogenous charge is second fluid nozzle, individual nozzle quantity is 2-6, Nozzle diameter is the second fluid nozzle of 5-15mm, and preferably, injection diameter is 8-10mm, this fluid tip requires can regulate each fluid flow rate easily, i.e. adjustable feed liquid flow, adjustable heated drying air flow, then adjustable spray atomization flow and effect.Such spray-drier can ensure more balanced by further for slip aerosol dispersion, make slip by equilibrium be distributed into main kiln after rapid crystallization dry.
Further, above-mentioned have in the spray-drier of Homogenizing pump homogenous charge regulate feed liquid flow to be 100mL/h-20 m
3/ h, the flow of kiln institute blowing air is 1-330m
3/ h, kiln internal pressure is 0.1-10bar, and the temperature of kiln and kiln institute blowing air is 90-200 DEG C.
In kiln, Sunmorl N 60S crystallite is adhered to fast to be continued crystallization and grows up, and crystallization and drying occur simultaneously, and are dried fast under hot blast condition.
(4) finished product is collected
Collect Sunmorl N 60S particle or micro mist.
Dry indoor hot air and material are evacuated to multi-cyclone and are separated by induced draft fan; the Sunmorl N 60S particle trapped bottom kiln, bottom cyclonic separator and in pocket type micro mist air filter or micro mist are collected collecting bin simultaneously; then make-up room is transported to, cooling weighing and bagging.
Beneficial effect of the present invention is as follows:
The present invention is applicable to the various production method gained sodium gluconate solutions of Sunmorl N 60S, as the sodium gluconate solution of double-enzyme method or the gained such as metal catalysed processes or fermentation method, once extracts, does not produce mother liquor, significantly reduces without decolouring cost or decolouring cost.As in the sodium gluconate solution that double-enzyme method or metal catalysed processes are produced without residual sugar or residual sugar content extremely low, product purity is high, color clarification color and luster is low, solution is refined without the need to gac etc. and can be applied extracting directly of the present invention, produces and do not produce decolouring cost after extracting without mother liquor.The Sunmorl N 60S of fermentative Production, the starting soln color and luster after filtering fermentation liquor thalline is not high, or only need not apply once a small amount of gac and can obtain clear soln, and employing the inventive method can extracting directly.And Sunmorl N 60S crystallization and drying complete in the present invention simultaneously, extract more direct, Production Flow Chart and greatly shorten.
The present invention obtains the balanced constant-pressure and high-temperature supersaturated solution of concentration distribution by controlling sodium gluconate solution with the ratio of Sunmorl N 60S crystal seed, also by control throw granularity, the degree of super saturation of crystal seed, homogenous charge, the spray orifice size of second fluid nozzle, drying air stream and supersaturated solution flow and jet velocity, make the Sunmorl N 60S entering kiln on crystal seed, adhere to condensation fast, form the gluconic acid sodium crystal of epigranular, full grains, product product are on very good terms.The speed that during spraying, Sunmorl N 60S is crystal formation is fast, also contributes to the energy consumption of auxiliary reduction drying tower endogenous pyrogen.
Embodiment
Further describe the present invention below in conjunction with specific embodiment, advantage and disadvantage of the present invention will be more clear along with description.But embodiment is only exemplary, does not form any restriction to scope of the present invention.It will be understood by those skilled in the art that and can modify to the details of technical solution of the present invention and form or replace down without departing from the spirit and scope of the present invention, but these amendments and replacement all fall within the scope of protection of the present invention.
Embodiment 1 one kinds does not generate the extracting method of the Sunmorl N 60S of mother liquor, and concrete steps are as follows
(1) strength of solution is modulated
Get and produce gained sodium gluconate solution (in this example, used pair of enzyme refers to glucose oxidase and catalase) by double-enzyme method Sunmorl N 60S, detecting residual sugar content is 0, and color and luster is clarified.Mass volume ratio clarification sodium gluconate solution being evaporated to dry-matter after simple filtration removal of impurities is 62%, and get 3L, be stored in and adjust in brilliant tank, temperature remains on 85 DEG C, constantly stirs and makes equalization of concentration.
(2) inoculate
Sunmorl N 60S crystal seed is inoculated in the solution of step (1) gained, inoculum size is the mass volume ratio of Sunmorl N 60S crystal seed and solution is 28%, i.e. 840g, stir after inoculation, rotating speed is 1150rpm/min, and temperature is 85.1 DEG C, and the time is 5min, mix, form the constant-pressure and high-temperature supersaturated solution of concentration distribution equilibrium.The Sunmorl N 60S crystal seed inoculated crosses 500 mesh sieves, and full grains, epigranular, sample after inoculation in 100ml graduated cylinder leave standstill 40 seconds time observe, the volume of crystal accounts for 27.7%, carries out crystallizing and drying.
(3) crystallizing and drying
Enable homogenous charge pump, open spray-drier, open induced draft fan and multi-cyclone.In this embodiment, spray-drier used is commercially available " Shunyi science and technology SP-1500 " laboratory spray drying machine.The rapid homogeneous of supersaturated solution step (2) obtained pumps into kiln and carries out spraying dry.The nozzle quantity of this spray-drier is 2, selected jet size is the second fluid nozzle of 2.0mm, and feed liquid flow is 1100mL/h, and kiln internal pressure is 4.2bar, the temperature of kiln and kiln institute blowing air is 110 ± 1 DEG C, and the flow of kiln institute blowing air is 3.5m
3/ h.
(4) finished product is collected
Dry indoor hot air and material are evacuated to multi-cyclone and are separated by induced draft fan, the Sunmorl N 60S particle of dry gained or micro mist bottom self-desiccation room and bottom cyclonic separator are collected simultaneously and are aggregated into collecting bin.From collecting bin, dried Sunmorl N 60S is transported to packaging chamber, cooling weighing vacuumizes and packs.Gained Sunmorl N 60S drying is weighed as 2706.1g, moisture content 0.3%, and the Sunmorl N 60S more than 95% is particulate state, and Sunmorl N 60S all reclaims, and produces without mother liquor.
Embodiment 2 one kinds does not generate the extracting method of the Sunmorl N 60S of mother liquor, and concrete steps are as follows
(1) strength of solution is modulated
Get and produce gained sodium gluconate solution (in this example, catalytic metal used is nanometer gold) by metal catalysed processes Sunmorl N 60S, detecting residual sugar content is 0, and color and luster is clarified.Mass volume ratio clarification sodium gluconate solution being evaporated to dry-matter after simple filtration removal of impurities is 53%, and get 3L, be stored in and adjust in brilliant tank, temperature remains on 65 DEG C, constantly stirs and makes equalization of concentration.
(2) inoculate
Sunmorl N 60S crystal seed is inoculated in the solution of step (1) gained, inoculum size is the mass volume ratio of Sunmorl N 60S crystal seed and solution is 12%, i.e. 360g, stir after inoculation, rotating speed is 550rpm/min, temperature is 65 DEG C, time is 4.5min, mix, form the constant-pressure and high-temperature supersaturated solution of concentration distribution equilibrium, the Sunmorl N 60S crystal seed inoculated crosses 200 mesh sieves, and full grains, granularity, observe when sampling standing 40 seconds in 100ml graduated cylinder after inoculation, the volume of crystal accounts for 24%, carries out crystallizing and drying.
(3) crystallizing and drying
Enable homogenous charge pump, open spray-drier, open induced draft fan and multi-cyclone.In this embodiment, spray-drier used is commercially available " Shunyi science and technology SP-1500 " laboratory spray drying machine.The rapid homogeneous of supersaturated solution step (2) obtained pumps into kiln and carries out spraying dry.The nozzle quantity of this spray-drier is 2, selected jet size is the second fluid nozzle of 2.0mm, and feed liquid flow is 800mL/h, and kiln internal pressure is 5.5bar, the temperature of kiln and kiln institute blowing air is 145 DEG C, and the flow of kiln institute blowing air is 4.5m
3/ h.
(4) finished product is collected
Dry indoor hot air and material are evacuated to multi-cyclone and are separated by induced draft fan, the Sunmorl N 60S particle of dry gained or micro mist bottom self-desiccation room and bottom cyclonic separator are collected simultaneously and are aggregated into collecting bin.From collecting bin, dried Sunmorl N 60S is transported to packaging chamber, cooling weighing vacuumizes and packs.Gained Sunmorl N 60S drying is weighed as 1955.2g, moisture content 0.4%, and the Sunmorl N 60S more than 92% is particulate state, and Sunmorl N 60S all reclaims, and produces without mother liquor.
Embodiment 3 one kinds does not generate the extracting method of the Sunmorl N 60S of mother liquor, and concrete steps are as follows
(1) strength of solution is modulated
Get and produce gained sodium gluconate solution by fermentation of Aspergillus niger method, detect residual sugar mass percentage content lower than 0.03%, color and luster is clarified.Mass volume ratio clarification sodium gluconate solution being evaporated to dry-matter after simple filtration removal of impurities is 66%, and get 3L, be stored in and adjust in brilliant tank, temperature remains on 88 DEG C, constantly stirs and makes equalization of concentration.
(2) inoculate
Sunmorl N 60S crystal seed is inoculated in the solution of step (1) gained, inoculum size is the mass volume ratio of Sunmorl N 60S crystal seed and solution is 37%, i.e. 1110g, stir after inoculation, rotating speed is 3200rpm/min, and temperature is 85.2 DEG C, and the time is 5min, mix, form the constant-pressure and high-temperature supersaturated solution of concentration distribution equilibrium.The Sunmorl N 60S crystal seed inoculated crosses 300 mesh sieves, and full grains, granularity, sample after inoculation in 100ml graduated cylinder leave standstill 40 seconds time observe, the volume of crystal accounts for 29.5%, carries out crystallizing and drying.
(3) crystallizing and drying
Enable homogenous charge pump, open spray-drier, open induced draft fan and multi-cyclone.In this embodiment, spray-drier used is commercially available " Shunyi science and technology SP-1500 " laboratory spray drying machine.The rapid homogeneous of supersaturated solution step (2) obtained pumps into kiln and carries out spraying dry.The nozzle quantity of this spray-drier is 2, selected jet size is the second fluid nozzle of 2.0mm, and feed liquid flow is 1800mL/h, and kiln internal pressure is 9bar, the temperature of kiln and kiln institute blowing air is 180 DEG C, and the flow of kiln institute blowing air is 9m
3/ h.
(4) finished product is collected
Dry indoor hot air and material are evacuated to multi-cyclone and are separated by induced draft fan, the Sunmorl N 60S particle of dry gained or micro mist bottom self-desiccation room and bottom cyclonic separator are collected simultaneously and are aggregated into collecting bin.From collecting bin, dried Sunmorl N 60S is transported to packaging chamber, cooling weighing vacuumizes and packs.Gained Sunmorl N 60S drying is weighed as 3094.9g, moisture content 0.21%, and the Sunmorl N 60S more than 93% is particulate state, and Sunmorl N 60S all reclaims, and produces without mother liquor.
Claims (9)
1. do not generate an extracting method for the Sunmorl N 60S of mother liquor, concrete steps are as follows:
(1) strength of solution is modulated
Evaporated by sodium gluconate solution after filtering and impurity removing, the mass volume ratio to dry-matter is 48-80%, and be then stored in and adjust brilliant tank, temperature is 62-90 DEG C, and constantly stirs;
(2) inoculate
Sunmorl N 60S crystal seed is inoculated in the solution of step (1) gained, inoculum size is the mass volume ratio of Sunmorl N 60S crystal seed and solution is 5-40%, stir after inoculation, rotating speed is 300-4000rpm/min, and temperature is 62-90 DEG C, and the time is 1-5min, mix, form the constant-pressure and high-temperature supersaturated solution of concentration distribution equilibrium, get supersaturated solution and leave standstill observation, carry out crystallizing and drying when the volume of crystal accounts for 20-30%;
(3) crystallizing and drying
Spraying dry is carried out in the kiln supersaturated solution that step (2) obtains being pumped into the spray-drier with Homogenizing pump homogenous charge;
(4) finished product is collected
Collect Sunmorl N 60S particle or micro mist.
2. extracting method according to claim 1, is characterized in that, in described step (1), the mass volume ratio of dry-matter is 50-65%, is stored in and adjusts the temperature in brilliant tank to be 85 DEG C.
3. extracting method according to claim 1, is characterized in that, the Sunmorl N 60S crystal seed of inoculation in described step (2) requires full grains, epigranular, and Sunmorl N 60S crystal seed crosses 100-500 mesh sieve.
4. extracting method according to claim 1, is characterized in that, in described step (2), inoculum size is 15-35%.
5. extracting method according to claim 1, is characterized in that, described step (2) medium speed is 1000-1200rmp/min.
6. extracting method according to claim 1, is characterized in that, after inoculating front and inoculation in described step (2), temperature all remains on 85 DEG C ± 0.5 DEG C.
7. extracting method according to claim 1, it is characterized in that, the nozzle in described step (3) with the spray atomization system of the spray-drier of Homogenizing pump homogenous charge is second fluid nozzle, and individual nozzle quantity is 2-6, and Nozzle diameter is the second fluid nozzle of 5-15mm.
8. extracting method according to claim 7, is characterized in that, in described step (3), injection diameter is 8-10mm.
9. extracting method according to claim 1, is characterized in that, has in the spray-drier of Homogenizing pump homogenous charge and regulate feed liquid flow to be 100mL/h-20 m in described step (3)
3/ h, the flow of kiln institute blowing air is 1-330m
3/ h, kiln internal pressure is 0.1-10bar, and the temperature of kiln and kiln institute blowing air is 90-200 DEG C.
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| CN201510182799.5A CN104829446A (en) | 2015-04-17 | 2015-04-17 | Method for extracting sodium gluconate without generating mother liquor |
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| CN201510182799.5A CN104829446A (en) | 2015-04-17 | 2015-04-17 | Method for extracting sodium gluconate without generating mother liquor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251998A (en) * | 2018-11-19 | 2019-01-22 | 潍坊盛泰药业有限公司 | A kind of particle glucose production method |
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|---|---|---|---|---|
| CN201678610U (en) * | 2010-02-09 | 2010-12-22 | 游汉生 | Gluconate spray drying system |
| CN102086149A (en) * | 2009-12-04 | 2011-06-08 | 西王集团有限公司 | Novel method for extracting sodium gluconate |
| CN103923953A (en) * | 2014-04-11 | 2014-07-16 | 山东省食品发酵工业研究设计院 | Method for solidifying sodium gluconate mother liquor produced by fermentation method |
| CN104450806A (en) * | 2014-11-27 | 2015-03-25 | 江南大学 | Method for preparing sodium gluconate with enzymatic method |
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2015
- 2015-04-17 CN CN201510182799.5A patent/CN104829446A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102086149A (en) * | 2009-12-04 | 2011-06-08 | 西王集团有限公司 | Novel method for extracting sodium gluconate |
| CN201678610U (en) * | 2010-02-09 | 2010-12-22 | 游汉生 | Gluconate spray drying system |
| CN103923953A (en) * | 2014-04-11 | 2014-07-16 | 山东省食品发酵工业研究设计院 | Method for solidifying sodium gluconate mother liquor produced by fermentation method |
| CN104450806A (en) * | 2014-11-27 | 2015-03-25 | 江南大学 | Method for preparing sodium gluconate with enzymatic method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109251998A (en) * | 2018-11-19 | 2019-01-22 | 潍坊盛泰药业有限公司 | A kind of particle glucose production method |
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Application publication date: 20150812 |