CN113003898B - Corn soaking water treatment method - Google Patents
Corn soaking water treatment method Download PDFInfo
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- CN113003898B CN113003898B CN202110444888.8A CN202110444888A CN113003898B CN 113003898 B CN113003898 B CN 113003898B CN 202110444888 A CN202110444888 A CN 202110444888A CN 113003898 B CN113003898 B CN 113003898B
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- C07F9/02—Phosphorus compounds
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- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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- C02F3/28—Anaerobic digestion processes
Abstract
The invention relates to the technical field of corn soaking water treatment, in particular to a corn soaking water treatment method, which comprises the following steps: (1) Enabling the supernatant after the corn is soaked in the water and kept stand to enter a cationic resin column, and collecting a first effluent and a second effluent; (2) The first effluent enters an anion resin column, the third effluent is collected, the second effluent enters the anion resin column, and the first section effluent with the pH value of 3.3 to neutral and the second section effluent with the pH value of less than 3.3 are respectively collected; (3) The first-stage effluent liquid is treated by ultrafiltration and nanofiltration, and trapped fluid is collected; (4) Filtering the third effluent collected in the step (2), fermenting the collected trapped fluid, and filtering the collected permeate through a nanofiltration membrane; by the treatment method, potassium ions in the corn soaking water can be recycled, the discharge amount of wastewater is reduced, and the consumption of potassium chloride raw materials for desorbing phytic acid is reduced.
Description
Technical Field
The invention relates to the technical field of corn soaking water treatment, in particular to a corn soaking water treatment method.
Background
In the corn starch wet milling production process, corn soaking water is used as main production wastewater, wherein the solid content is about 10-12%, and the corn soaking water contains substances such as 5-6% of protein, 2-3% of lactic acid, 1% of phytic acid, 1% of sugar, a small amount of starch residue, inorganic salt and the like, and the conventional treatment modes of the corn soaking water at present mainly comprise the following two modes: (1) Corn steep water is evaporated and concentrated from 6 to 10 percent to 40 percent of corn steep liquor through a multi-effect evaporator, the corn steep liquor is directly sold or sprayed for sale, but the price fluctuation of the corn steep liquor is large due to the influence of seasons or purchasers, and the treatment cost of high COD sewage exists; (2) The corn soaking water is used for producing protein powder, but because the components in the corn soaking water are complex, the corn soaking water contains protein components, small molecular sugar, (sulfite) sulfate, pigment and the like, and even aflatoxin, the corn soaking water is directly used for producing the protein powder, the quality of products is poor, and food or other safety risks also exist; (3) In order to effectively utilize components in the corn soaking water, the prior treatment process adopts a process method of treating the corn soaking water to obtain products such as inositol, protein, lactic acid and the like; when the phytic acid is desorbed, newly prepared potassium chloride solution is used as a desorbent, and the corn soaking water contains potassium ions, but the potassium ions are not recycled by the conventional process method, so that the resource waste is caused, and in addition, the operation process for preparing the lactic acid is complicated, the cost is high, and the wastewater is easily generated. Therefore, in order to solve the above problems, there is a need to establish a method for treating corn steep water.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects in the prior art, the method for treating the corn soaking water is provided, potassium ions in the corn soaking water can be recycled by the method, the discharge amount of wastewater is reduced, and the consumption of a potassium chloride raw material for desorbing phytic acid is reduced.
In order to solve the technical problem, the technical scheme of the invention is as follows:
a corn steep water treatment method comprises the following steps:
(1) Allowing the supernatant of the corn soaking water after standing to enter a cation resin column, collecting a first effluent for later use, washing the cation resin column with hydrochloric acid, and collecting a second effluent for later use;
(2) Enabling the first effluent obtained in the step (1) to enter an anion resin column, collecting a third effluent for later use, enabling the second effluent obtained in the step (1) to serve as a desorbent to enter the anion resin column, and respectively collecting a first-stage effluent with the pH value of 3.3 to neutral and a second-stage effluent with the pH value of less than 3.3;
(3) Performing ultrafiltration and nanofiltration treatment on the first-stage effluent liquid collected in the step (2), wherein the collected trapped liquid is a potassium phytate solution; taking the second-stage effluent collected in the step (2) as a desorbent of the next batch of the cationic resin column, and introducing the second-stage effluent into the cationic resin column, wherein the collected effluent is used as a desorbent component of the next batch of the anionic resin column in the step (2);
(4) Filtering the third effluent collected in the step (2) by using an ultrafiltration membrane, fermenting the collected trapped fluid, filtering the collected permeate by using a nanofiltration membrane, and respectively collecting the trapped fluid and the permeate for later use;
(5) Spray drying the trapped fluid for later use in the step (4) to obtain a corn protein powder product; treating the reserved permeate with a reverse osmosis membrane, and respectively collecting the trapped fluid and the permeate for later use;
(6) Carrying out vacuum concentration and vacuum distillation treatment on the trapped liquid collected in the step (5) to obtain a lactic acid product; and (4) mechanically applying the permeate collected in the step (5) as process production water.
As an improved technical scheme, the resin in the cation resin column in the step (1) is strong acid cation resin, the type of the resin is Hairun HAD-10 resin, and the volume of the resin in the cation resin column is 3BV.
As a modified means, the concentration of the hydrochloric acid in the step (1) is 8% -10% w/v, the volume of the hydrochloric acid is 1.3-2 times the volume of the resin in the cationic resin column, and the hydrochloric acid is introduced into the cationic resin column at a flow rate of 0.5 BV/h.
As an improved technical scheme, the resin in the anion resin column in the step (2) is a weak base anion exchange resin, and the type of the resin is weak base acrylic resin ZG312.
As an improved technical scheme, fermentation strains are added when the trapped fluid collected in the step (4) is fermented, the mixture is stirred for 10-15min every 3h, the fermentation temperature is maintained at 30-50 ℃, and the mixture is fermented and stirred for 7-10 days.
As an improved technical scheme, the molecular weight cut-off of the ultrafiltration membrane is 10-20 ten thousand, the molecular weight cut-off of the nanofiltration membrane is 500-600, and the molecular weight cut-off of the reverse osmosis membrane is less than 100.
As an improved technical scheme, the corn soaking water in the step (1) is kept stand for 4-6h at the temperature of 45-50 ℃.
After the technical scheme is adopted, the invention has the beneficial effects that:
the treatment method comprises the steps of adsorbing supernatant obtained after standing corn soaking water through a cation resin column, desorbing the cation resin column through hydrochloric acid, enabling obtained mixed solution of potassium chloride and hydrochloric acid to enter an anion resin column for desorbing phytic acid, respectively collecting first-stage effluent liquid with the pH value of 3.3 to be neutral and second-stage effluent liquid with the pH value of less than 3.3, and collecting trapped liquid obtained after ultrafiltration and nanofiltration of the first-stage effluent liquid to be potassium phytate solution; the effluent liquid of the second section is used as the desorbent component of the next batch of the cation resin column again, and the collected effluent liquid is used as the desorbent component of the next batch of the anion resin column; the process method realizes the recycling of potassium ions in the corn soaking water, greatly reduces the consumption of potassium chloride for desorbing the phytic acid, has simple operation in the whole process, does not need other operations such as membrane filtration on the effluent liquid after the desorption of the cation resin column, and does not need regeneration treatment on the cation resin column by alkali liquor; the treatment method of the invention intercepts and ferments the crude protein in the corn soaking water, and the crude protein is sold as a product; the treatment method of the invention recovers the lactic acid in the corn soaking water, adopts ultrafiltration, nanofiltration and reverse osmosis operation, and has simple and convenient operation; the treatment method comprises the steps of adsorbing the first effluent after the effluent passes through the cation resin column by the anion resin column, desorbing by using potassium chloride, and carrying out a series of treatments on the collected desorption solution to obtain inositol and high-value byproducts. The whole treatment method also recycles the wastewater, and saves water. The processing method fully utilizes the components of the corn soaking water, does not waste any resources, obtains a plurality of products, and greatly brings economic benefits to enterprises.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A corn soaking water treatment method comprises the following steps:
(1) Standing corn soaking water at 45-50 deg.C for 4h to obtain supernatant 650L, feeding into 135L cationic resin column (strong acid type cationic resin Hai run HAD-10, resin volume in cationic resin column is 3 BV) at a flow rate of 1.2BV/h, collecting first effluent, washing the cationic resin column with 8 w/v, 180L hydrochloric acid solution at 0.5BV/h, and collecting second effluent;
(2) Enabling the first effluent obtained in the step (1) to enter an anion resin column (a filler in the resin column is gel-type weakly alkaline acrylic resin ZG 312), collecting a third effluent for later use, enabling the third effluent to enter the anion resin column by taking the second effluent obtained in the step (1) as a desorbent, and respectively collecting 75L (a mixed solution of potassium phytate and potassium chloride) of a first-stage effluent with the pH value of 3.3 to neutral and 75L (a mixed solution of phytic acid and hydrochloric acid) of a second-stage effluent with the pH value of less than 3.3, and supplementing the first-stage effluent to 180L by using newly-prepared hydrochloric acid;
(3) Performing ultrafiltration (ultrafiltration membrane with molecular weight cut-off of 10-20 ten thousand) and nanofiltration treatment (nanofiltration membrane with molecular weight cut-off of 800-1000) on the first-stage effluent collected in the step (2), wherein the collected cut-off solution is 18L of potassium phytate solution (the content of potassium phytate is 25%); taking the second-stage effluent collected in the step (2) as a desorbent of the next batch of the cation resin column, and introducing the second-stage effluent into the cation resin column, wherein the collected effluent is used as a desorbent component of the next batch of the anion resin column;
(4) Filtering 650L of the third effluent collected in step (2) with ultrafiltration membrane with cut-off molecular weight of 10-20 ten thousand, fermenting the collected cut-off 50L of cut-off solution with solid content of 18 w/v (the added strain is EM microbial inoculum, the addition amount is 0.05% w/v, the strain is purchased from manufacturer), stirring for 10-15min every 3h, maintaining the fermentation temperature at 30-50 deg.C, fermenting and stirring for 7-10 days, wherein the organic matter content of the solid content of the obtained fermented product reaches 40%, and the bacterial content reaches more than 5000/g. ) Filtering 600L of the collected permeation solution by a nanofiltration membrane with the molecular weight cutoff of 500, and respectively collecting the trapped solution and the permeation solution for later use;
(5) Treating 120L of trapped fluid for later use in the step (4) until the solid content reaches 30% (w/v) by spray drying (the air inlet temperature is 130 ℃, the air outlet temperature is 95 ℃) to obtain a corn protein powder product; treating 480L of the permeate for later use by a reverse osmosis membrane (the molecular weight cut-off is less than 100), and respectively collecting the cut-off liquid and the permeate for later use;
(6) 240L of trapped liquid collected in the step (5) enters a distillation still with the pressure of-0.09 to-0.095 Mpa, temperature rising distillation is carried out, water with a low boiling point is collected independently until no distillation is carried out, the vacuum degree is improved until the vacuum is stabilized at the absolute pressure of 100Pa, temperature rising distillation is carried out, about 200L of water with the temperature lower than 55 ℃ is collected independently, then a fraction collection tank is switched to collect fractions at the temperature of 82-85 ℃/100Pa, and distillation is carried out until no distillation is carried out, so that 22kg of lactic acid aqueous solution with the lactic acid content of 50% is obtained; adding 20L of water into the kettle bottom dry matter, heating, boiling, discharging, and drying to obtain 15kg; and (4) mechanically applying 240L of permeate collected in the step (5) as process production water.
Example 2
A corn soaking water treatment method comprises the following steps:
(1) Standing corn soaking water at 45-50 deg.C for 5h to obtain supernatant 650L, feeding into 135L cationic resin column (strong acid type cationic resin Hai run HAD-10, resin volume in cationic resin column is 3 BV) at a flow rate of 1.2BV/h, collecting first effluent, washing the cationic resin column with 9 w/v, 180L hydrochloric acid solution at 0.5BV/h, and collecting second effluent;
(2) Allowing the first effluent collected in the step (1) to enter an anion resin column (the filler in the resin column is gel-type weakly alkaline acrylic resin ZG 312), collecting a third effluent for later use, allowing the second effluent obtained in the step (1) to enter the anion resin column by taking the second effluent as a desorbent, and respectively collecting a first-stage effluent (a mixed solution of potassium phytate and potassium chloride) with the pH value of 3.3 to neutrality and a second-stage effluent (a mixed solution of phytic acid and hydrochloric acid) with the pH value of less than 3.3;
(3) Performing ultrafiltration (ultrafiltration membrane with molecular weight cut-off of 10-20 ten thousand) and nanofiltration treatment (nanofiltration membrane with molecular weight cut-off of 800) on the first-stage effluent collected in the step (2), wherein the collected trapped liquid is 19L of potassium phytate solution (the content of potassium phytate is 26%); taking the second-stage effluent collected in the step (2) as a desorbent of the next batch of the cation resin column, and entering the cation resin column, wherein the collected effluent is used as a desorbent component of the next batch of the anion resin column in the step (2);
(4) Filtering 650L of the third effluent collected in the step (2) by an ultrafiltration membrane with the molecular weight cut-off of 10-20 ten thousand, performing fermentation treatment on 50L of the collected cut-off solution with the solid content of 18 w/v (the added strain is EM microbial inoculum, the addition amount is 0.05 percent w/v), stirring for 10-15min every 3h, maintaining the fermentation temperature at 30-50 ℃, and performing fermentation stirring for 7-10 days, wherein the organic matter content of the solid content of the obtained fermentation product reaches 40 percent, and the bacterial content reaches more than 5000/g. ) Filtering 600L of the collected permeation solution by a nanofiltration membrane with the molecular weight cutoff of 500, and respectively collecting the trapped solution and the permeation solution for later use;
(5) Treating 120L of retentate prepared in the step (4) until the solid content reaches 30% (w/v) by spray drying (the air inlet temperature is 130 ℃, the air outlet temperature is 95 ℃) to obtain a corn protein powder product; treating 480L of the reserved permeate through a reverse osmosis membrane (the molecular weight cut-off is less than 100), and respectively collecting the cut-off and the permeate for later use;
(6) Allowing 240L of trapped liquid collected in the step (5) to enter a distillation still with the pressure of-0.09 to-0.095 Mpa, heating for distillation, separately collecting water with a low boiling point until no distillation, increasing the vacuum degree to be vacuum stable at 100Pa, heating for distillation, separately collecting about 200L of water with the temperature lower than 55 ℃, switching a fraction collection tank to collect fractions with the temperature of 82-85 ℃/100Pa, and distilling until no distillation, so as to obtain 22kg of lactic acid aqueous solution with the lactic acid content of 50%; adding 20L of water into the dry matter at the bottom of the kettle, heating, boiling, discharging and drying to obtain 15kg; and (4) mechanically applying 240L of permeate collected in the step (5) as process production water.
Example 3
A corn soaking water treatment method comprises the following steps:
(1) Standing corn soaking water at 45-50 deg.C for 6h to obtain supernatant 650L, feeding into 135L cationic resin column (strong acid type cationic resin Hai run HAD-10, resin volume in cationic resin column is 3 BV) of resin filler at a flow rate of 1.2BV/h, collecting first effluent, washing the cationic resin column with 10 w/v, 180L hydrochloric acid solution at 0.5BV/h, and collecting second effluent;
(2) Enabling the first effluent collected in the step (1) to enter an anion resin column (the filler in the resin column is gel type weakly alkaline acrylic resin ZG312, the volume of the anion resin column is 45L), collecting a third effluent for later use, enabling the second effluent in the step (1) to serve as a desorbent to enter the anion resin column, and respectively collecting a first-stage effluent (a mixed solution of potassium phytate and potassium chloride, the first 26L and the subsequent 75L) with the pH value of 3.3 to be neutral and a second-stage effluent (a mixed solution of phytic acid and hydrochloric acid, the first 154L and the subsequent 105L) with the pH value of less than 3.3;
(3) Performing ultrafiltration (ultrafiltration membrane with molecular weight cut-off of 10-20 ten thousand) and nanofiltration treatment (nanofiltration membrane with molecular weight cut-off of 800-1000) on the first-stage effluent collected in the step (2), wherein the collected cut-off solution is 20L of potassium phytate solution (the content of potassium phytate is 27%); taking the second-stage effluent collected in the step (2) as a desorbent of the next batch of the cation resin column, and introducing the second-stage effluent into the cation resin column, wherein the collected effluent is used as a desorbent component of the next batch of the anion resin column;
(4) Filtering 650L of the third effluent collected in the step (3) by an ultrafiltration membrane with the molecular weight cut-off of 10-20 ten thousand, performing fermentation treatment on 50L of the collected cut-off solution with the solid content of 18 w/v (the added strain is EM microbial inoculum, the addition amount is 0.05 percent w/v), stirring for 10-15min every 3h, maintaining the fermentation temperature at 30-50 ℃, and performing fermentation stirring for 7-10 days, wherein the organic matter content of the solid content of the obtained fermentation product reaches 40 percent, and the bacterial content reaches more than 5000/g. ) Filtering 600L of the collected permeate through a nanofiltration membrane with the molecular weight cutoff of 500, and respectively collecting the cutoff liquid and the permeate for later use;
(5) Treating 120L of trapped fluid for later use in the step (4) until the solid content reaches 30% (w/v) by spray drying (the air inlet temperature is 130 ℃, the air outlet temperature is 95 ℃) to obtain a corn protein powder product; treating 480L of the reserved permeate through a reverse osmosis membrane (the molecular weight cut-off is less than 100), and respectively collecting the cut-off and the permeate for later use;
(6) Allowing 240L of trapped liquid collected in the step (5) to enter a distillation still with the pressure of-0.09 to-0.095 Mpa, heating for distillation, separately collecting water with a low boiling point until no distillation, increasing the vacuum degree to be vacuum stable at 100Pa, heating for distillation, separately collecting about 200L of water with the temperature lower than 55 ℃, collecting fractions at the temperature of 82-85 ℃/100Pa, and distilling until no distillation to obtain 22kg of lactic acid aqueous solution with the lactic acid content of 50%; adding 20L of water into the dry matter at the bottom of the kettle, heating, boiling, discharging and drying to obtain 15kg; and (4) mechanically applying 240L of permeate collected in the step (5) as process production water.
To better demonstrate the advantages of the treatment method of the invention with respect to the prior art, the following 2 comparative examples are given, the specific experimental results of which are given in table 1.
Comparative example 1
Different from the embodiment 1, the supernatant fluid of the corn soaking water after standing is not absorbed by a cation resin column, but directly enters an anion resin column, the effluent liquid is subjected to ultrafiltration, nanofiltration and reverse osmosis operation (the treatment mode is the same as the embodiment 1), and the anion resin column is subjected to desorption treatment by potassium chloride solution (the treatment mode is the same as the embodiment 1);
comparative example 2
The difference from the example 1 is that the supernatant fluid of the corn soaking water after standing is not absorbed by a cation resin column, but directly enters an anion resin column, the effluent liquid is subjected to ultrafiltration and nanofiltration operations (the treatment mode is the same as the example 1), and the anion resin column is desorbed by potassium chloride solution (the treatment mode is the same as the example 1);
TABLE 1
The data in table 1 show that the process method provided by the invention realizes the recycling of potassium in the corn soaking water, the potassium chloride raw material is not consumed during the desorption of phytic acid in the examples 1 to 3, the zero discharge of wastewater is realized in the whole process, the consumption of the potassium chloride raw material is greatly reduced compared with the comparative examples 1 and 2, the resource waste is avoided, and the zero discharge of wastewater is also realized.
Here, it should be noted that the data in Table 1 are the data in Table 1 obtained by determining the corn steep water content of the batch 10.8% w/v, the protein content 5.2% w/v, the lactic acid 2.3% w/v, the phytic acid 1.01% w/v, such that the phytic acid content of 10.1kg of potassium phytate 13.59kg, the protein content of 52kg, and the lactic acid content of 23.9kg were calculated in 1000L of corn steep water.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (7)
1. A corn soaking water treatment method is characterized by comprising the following steps:
(1) Allowing supernatant of the corn soaking water after standing to enter a cation resin column, collecting a first effluent for later use, washing the cation resin column by using hydrochloric acid, and collecting a second effluent for later use;
(2) Enabling the first effluent obtained in the step (1) to enter an anion resin column, collecting a third effluent for later use, enabling the second effluent obtained in the step (1) to serve as a desorbent to enter the anion resin column, and respectively collecting a first-stage effluent with the pH value of 3.3 to neutral and a second-stage effluent with the pH value of less than 3.3;
(3) Performing ultrafiltration and nanofiltration treatment on the first-stage effluent collected in the step (2), wherein the collected trapped fluid is a potassium phytate solution; taking the second-stage effluent collected in the step (2) as a desorbent of the next batch of the cationic resin column, and introducing the second-stage effluent into the cationic resin column, wherein the collected effluent is used as a desorbent component of the next batch of the anionic resin column in the step (2);
(4) Filtering the third effluent collected in the step (2) by using an ultrafiltration membrane, fermenting the collected trapped fluid, filtering the collected permeate by using a nanofiltration membrane, and respectively collecting the trapped fluid and the permeate for later use;
(5) Spray drying the trapped fluid for later use in the step (4) to obtain a corn protein powder product; treating the reserved permeate with a reverse osmosis membrane, and respectively collecting the trapped fluid and the permeate for later use;
(6) Carrying out vacuum concentration and vacuum distillation treatment on the trapped liquid collected in the step (5) to obtain a lactic acid product; and (4) mechanically applying the permeate collected in the step (5) as process production water.
2. The corn steep water treatment method according to claim 1, characterized in that: the resin in the cation resin column in the step (1) is strong acid cation resin, the type of the resin is Hairun HAD-10 resin, and the volume of the resin in the cation resin column is 3BV.
3. The corn steep water treatment method according to claim 1, characterized in that: the concentration of the hydrochloric acid in the step (1) is 8% -10% w/v, the volume of the hydrochloric acid is 1.3-2 times the volume of the resin in the cationic resin column, and the hydrochloric acid is introduced into the cationic resin column at a flow rate of 0.5 BV/h.
4. The corn steep water treatment method according to claim 1, characterized in that: and (3) in the step (2), the resin in the anion resin column is a weak base anion exchange resin, and the type of the resin is weak base acrylic resin ZG312.
5. The corn steep water treatment method according to claim 1, characterized in that: adding fermentation strains when the trapped fluid collected in the step (4) is fermented, stirring for 10-15min every 3h, maintaining the fermentation temperature at 30-50 ℃, and fermenting and stirring for 7-10 days.
6. The corn steep water treatment method according to claim 1, characterized in that: the molecular weight cut-off of the ultrafiltration membrane is 10-20 ten thousand, the molecular weight cut-off of the nanofiltration membrane is 500-600, and the molecular weight cut-off of the reverse osmosis membrane is less than 100.
7. The corn steep water treatment method according to claim 1, characterized in that: standing the corn soaking water in the step (1) for 4-6h at the temperature of 45-50 ℃.
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| CN113980047B (en) * | 2021-10-15 | 2023-08-18 | 山东寿光巨能金玉米开发有限公司 | Preparation method of phytic acid |
| CN114591362A (en) * | 2022-04-01 | 2022-06-07 | 诸城市浩天药业有限公司 | Novel process for preparing phytoacid |
| CN114604937B (en) * | 2022-04-01 | 2023-11-28 | 诸城市浩天药业有限公司 | Potassium phytate production process |
| CN115212985A (en) * | 2022-06-22 | 2022-10-21 | 江苏力德尔电子信息技术有限公司 | Polylactic acid modified plastic preparation facilities |
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