Process method for producing potassium hydrogen tartrate by using corn soaking water

Abstract

The invention discloses a process method for producing potassium hydrogen tartrate by using corn soaking water, and relates to the technical field of corn soaking water utilization, the corn soaking water is settled and then enters an anion exchange resin column, tartaric acid is added into effluent, diluted hydrochloric acid is added into a potassium hydrogen tartrate crude product obtained after reaction, stirring and dissolving are carried out, then filtering is carried out, activated carbon is added for decoloration, and the potassium hydrogen tartrate crude product is obtained; and adding alkali to neutralize the generated potassium hydrogen tartrate precipitate, and centrifuging and drying to obtain a finished product of potassium hydrogen tartrate. The potassium ions in the corn soaking water can be conveniently and quickly recovered, the potassium resource in the corn soaking water is fully recovered, and a new way for regenerating the potassium resource is opened up. Compared with a traditional method for recovering potassium ions by using cationic resin, the method has the advantages of small equipment investment and low operation cost.

Description

Technical Field

[0001] The invention relates to the technical field of corn soaking water utilization, and in particular to a process for producing potassium hydrogen tartrate by utilizing corn soaking water. Background Art

[0002] Potassium is a key element essential for plant growth. Potassium fertilizer promotes robust plant growth, strong stems, enhances resistance to pests and diseases, and promotes the production of sugars and starch. However, my country's potassium resources are in short supply, low in quality, and expensive to mine. Consequently, large quantities of potassium fertilizer must be imported annually to meet domestic agricultural production needs.

[0003] Corn soaking water, a waste product from the wet-process corn starch production process, is rich in potassium. Fully utilizing the potassium in this water would significantly alleviate my country's potassium shortage and generate significant economic and social benefits.

[0004] Currently, potassium recovery from corn soak water is mostly achieved through a cationic resin exchange method. This involves using a cationic resin to absorb potassium ions from the corn soak water, followed by acid desorption to produce an acidic solution containing potassium ions. This solution is then separated, concentrated, and crystallized to produce the potassium product. This current process, however, suffers from significant equipment investment, lengthy processes, and high production costs, limiting the potential for potassium recovery from corn soak water. Summary of the Invention

[0005] The technical problem to be solved by the present invention is: in view of the shortcomings of the existing technology, a process for producing potassium hydrogen tartrate by utilizing corn soaking water is provided, which is simple and has a high yield of potassium element.

[0006] In order to solve the above technical problems, the technical solution of the present invention is:

[0007] A process for producing potassium hydrogen tartrate using corn soaking water comprises the following steps:

[0008] A: After the corn soaking water is allowed to settle, the clear liquid is collected for later use. After the suspended matter settles, it is returned to the starch factory to be used to prepare corn starch powder.

[0009] B: The clear liquid enters the anion exchange resin column to absorb the phytic acid in the corn soaking water, and the effluent is reserved;

[0010] C: Add tartaric acid to the effluent to adjust the pH to 1.5-2.5. Potassium reacts with tartaric acid to form potassium hydrogen tartrate precipitate, which is filtered to obtain crude potassium hydrogen tartrate;

[0011] D: Add dilute hydrochloric acid solution to the crude potassium hydrogen tartrate, stir to dissolve, filter to remove denatured protein precipitate, then add activated carbon for decolorization, and filter to obtain a decolorized solution;

[0012] E: Add alkali to neutralize the decolorized solution to produce potassium hydrogen tartrate precipitate, which is then centrifuged and filtered to obtain the wet potassium hydrogen tartrate product;

[0013] F: Wet potassium hydrogen tartrate, which is dried to obtain finished potassium hydrogen tartrate.

[0014] Preferably, the suspended matter in step A is returned to the starch factory after sedimentation to prepare corn yellow powder.

[0015] Preferably, the anion exchange resin column in step B is a strongly basic macroporous anion exchange resin column, with a feed volume of 8-12 BV and a feed rate of 1-3 BV / h.

[0016] Preferably, the anion exchange resin column after adsorption of phytic acid in step B is eluted with an eluting agent, and the eluted solution is concentrated and then directly sold or hydrolyzed to produce inositol and by-products;

[0017] The analytical agent is one of HCl solution, KCl solution, KOH solution, NaCl solution and NaOH solution. The concentration of the analytical agent is 4-15% wt, the dosage is 1.5-2.5 BV, and the analytical flow rate is 1-3 BV / h.

[0018] Preferably, the reaction temperature in step C is 10-20° C., and the filtrate after filtration is returned to the starch factory to prepare corn yellow powder.

[0019] Preferably, the concentration of dilute hydrochloric acid in step D is 5-8 wt %, and the weight ratio of dilute hydrochloric acid to crude potassium hydrogen tartrate is 2-3:1.

[0020] Preferably, the stirring temperature in step D is 30-50°C, the amount of activated carbon used is 3-5‰wt, and the decolorization time is 0.5-1h.

[0021] Preferably, the denatured protein precipitate in step D is dried and used as protein feed.

[0022] Preferably, the mother liquor from the centrifugation in step E is recycled to be used as a decomposing agent after the anion exchange resin column adsorbs phytic acid in step B or to recover potassium chloride.

[0023] Preferably, the base in step E is a KOH solution with a concentration of 5-35% wt, and the pH of the solution after neutralization is 1.5-2.5.

[0024] Due to the adoption of the above technical solution, the beneficial effects of the present invention are:

[0025] 1. By adding tartaric acid to the corn soaking water, potassium ions in the corn soaking water react with tartaric acid to form potassium hydrogen tartrate precipitate. This method can quickly and easily recover potassium ions from the corn soaking water, fully recovering the potassium resources in the corn soaking water and opening up a new path for potassium resource regeneration. Compared with traditional cationic resin methods for recovering potassium ions, this method requires less equipment investment and has lower operating costs.

[0026] 2. Potassium hydrogen tartrate crude product is mixed with impurities such as protein and pigment from corn soaking water. In order to improve product quality and facilitate the dissolution of potassium hydrogen tartrate in acid, and the characteristic of protein denaturation when encountering acid, the crude tartaric acid solution is eluted in acid solution, the denatured protein precipitate is removed by filtration, and then the pigment in the filtrate is removed with activated carbon, thereby removing impurities in the crude tartaric acid and improving its purity.

[0027] 3. The production process of the present invention generates less three wastes and has little impact on the environment. In addition, the intermediate waste can be used for the production of corn yellow meal and protein feed, thereby improving economic benefits. DETAILED DESCRIPTION

[0028] The present invention will be further described below with reference to the embodiments.

[0029] Example 1

[0030] A process for producing potassium hydrogen tartrate using corn soaking water comprises the following steps:

[0031] A: 100L corn soaking water (potassium ion content 6‰wt) was allowed to settle and the clear liquid was collected for later use. After the suspended matter settled, it was returned to the starch factory to prepare corn yellow powder.

[0032] B: The clear liquid enters the anion exchange resin column to absorb the phytic acid in the corn soaking water. 100L of the effluent is reserved. The anion exchange resin column is a strong alkaline macroporous anion exchange resin column with a feed volume of 8BV and a feed rate of 1BV / h.

[0033] The anion exchange resin column after adsorption of phytic acid is analyzed with an analytical agent, and the 19L analytical solution is concentrated and then directly sold or hydrolyzed to produce inositol and by-products;

[0034] The analytical agent is HCl solution, the analytical agent concentration is 4% wt, the dosage is 1.5 BV, and the analytical flow rate is 1 BV / h;

[0035] C: Tartaric acid is added to the effluent to adjust the pH to 2.5. Potassium reacts with tartaric acid at 10°C to form potassium hydrogen tartrate precipitate. 4500 g of crude potassium hydrogen tartrate is obtained by filtration. 100 L of the filtered filtrate is returned to the starch factory to prepare corn yellow powder.

[0036] D: Add 5wt% dilute hydrochloric acid solution to the crude potassium hydrogen tartrate, stir and dissolve at 30°C, filter to remove the denatured protein precipitate, then add 3‰wt% activated carbon for decolorization for 0.5h, filter to obtain 11L of decolorized solution, wherein the weight ratio of dilute hydrochloric acid to crude potassium hydrogen tartrate is 2:1. After drying, 200g of the denatured protein precipitate is used as protein feed, activated carbon;

[0037] E: The decolorized liquid was neutralized to a pH of 1.5 by adding a 5% wt KOH solution to produce potassium hydrogen tartrate precipitate, which was centrifuged to obtain a wet product of potassium hydrogen tartrate. 11.5 L of the mother liquor was centrifuged and concentrated to recover potassium chloride crystals;

[0038] F: Wet potassium hydrogen tartrate was dried to obtain 2500 g of finished potassium hydrogen tartrate with a purity of 99.5% and a yield of 86.5%.

[0039] Example 2

[0040] A process for producing potassium hydrogen tartrate using corn soaking water comprises the following steps:

[0041] A: 100L corn soaking water (potassium ion content 6‰wt) was allowed to settle and the clear liquid was collected for later use. After the suspended matter settled, it was returned to the starch factory to prepare corn yellow powder.

[0042] B: The clear liquid enters the anion exchange resin column to absorb the phytic acid in the corn soaking water. 100L of the effluent is reserved. The anion exchange resin column is a strong alkaline macroporous anion exchange resin column with a feed volume of 10BV and a feed rate of 2BV / h.

[0043] The anion exchange resin column after adsorption of phytic acid is analyzed with an analytical agent, and 20L of the analytical solution is concentrated and then directly sold or hydrolyzed to produce inositol and by-products;

[0044] The analytical agent is KCl solution, the analytical agent concentration is 8% wt, the dosage is 2BV, and the analytical flow rate is 2BV / h;

[0045] C: Tartaric acid was added to the effluent to adjust the pH to 2. Potassium reacted with tartaric acid at 15°C to form potassium hydrogen tartrate precipitate. 4700 g of crude potassium hydrogen tartrate was obtained by filtration. 100 L of the filtered filtrate was returned to the starch factory to prepare corn yellow powder.

[0046] D: Add 6wt% dilute hydrochloric acid solution to the crude potassium hydrogen tartrate, stir and dissolve at 40°C, filter to remove the denatured protein precipitate, then add 4‰wt% activated carbon for decolorization for 0.8h, filter to obtain 12.5L of decolorized solution, wherein the weight ratio of dilute hydrochloric acid to crude potassium hydrogen tartrate is 2.5:1. After drying, 280g of the denatured protein precipitate is used as protein feed, activated carbon;

[0047] E: The decolorized solution was neutralized to pH 2 by adding 15% wt KOH solution to produce potassium hydrogen tartrate precipitate, which was centrifuged to obtain a wet potassium hydrogen tartrate product. 13 L of the mother liquor was recycled and used as the analytical reagent after the anion exchange resin column adsorbed phytic acid in step B;

[0048] F: Wet potassium hydrogen tartrate was dried to obtain 2550 g of finished potassium hydrogen tartrate with a purity of 99.3% and a yield of 88.2%.

[0049] Example 3

[0050] A process for producing potassium hydrogen tartrate using corn soaking water comprises the following steps:

[0051] A: 100L corn soaking water (potassium ion content 6‰wt) was allowed to settle and the clear liquid was collected for later use. After the suspended matter settled, it was returned to the starch factory to prepare corn yellow powder.

[0052] B: The clear liquid enters the anion exchange resin column to absorb the phytic acid in the corn soaking water. 100L of the effluent is reserved. The anion exchange resin column is a strong alkaline macroporous anion exchange resin column with a feed volume of 10BV and a feed rate of 2BV / h.

[0053] The anion exchange resin column after adsorption of phytic acid is analyzed with an analytical agent, and 25L of the analytical solution is concentrated and then directly sold or hydrolyzed to produce inositol and by-products;

[0054] The analytical agent is KOH solution, the analytical agent concentration is 12% wt, the dosage is 2.5 BV, and the analytical flow rate is 3 BV / h;

[0055] C: Tartaric acid was added to the effluent to adjust the pH to 1.5. Potassium reacted with tartaric acid at 20°C to form potassium hydrogen tartrate precipitate. 5200 g of crude potassium hydrogen tartrate was obtained by filtration. 100 L of the filtered filtrate was returned to the starch factory to prepare corn yellow powder.

[0056] D: Add 8wt% dilute hydrochloric acid solution to the crude potassium hydrogen tartrate, stir and dissolve at 50°C, filter to remove denatured protein precipitate, then add 5‰wt% activated carbon for decolorization for 1 hour, filter to obtain 17.5L of decolorized solution, wherein the weight ratio of dilute hydrochloric acid to crude potassium hydrogen tartrate is 3:1. After drying, 350g of the denatured protein precipitate is used as protein feed, activated carbon;

[0057] E: The decolorized liquid was neutralized to pH 2.5 by adding a 25% wt KOH solution to produce potassium hydrogen tartrate precipitate, which was centrifuged to obtain a wet potassium hydrogen tartrate product. 17.5 L of the mother liquor was concentrated and potassium chloride crystals were recovered.

[0058] F: Wet potassium hydrogen tartrate was dried to obtain 2610 g of finished potassium hydrogen tartrate with a purity of 99.3% and a yield of 90.3%.

[0059] Example 4

[0060] A process for producing potassium hydrogen tartrate using corn soaking water comprises the following steps:

[0061] A: 100L corn soaking water (potassium ion content 6‰) was allowed to settle and the clear liquid was collected for later use. After the suspended matter settled, it was returned to the starch factory to prepare corn yellow powder.

[0062] B: The clear liquid enters the anion exchange resin column to absorb the phytic acid in the corn soaking water. 100L of the effluent is reserved. The anion exchange resin column is a strong alkaline macroporous anion exchange resin column with a feed volume of 12BV and a feed rate of 3BV / h.

[0063] The anion exchange resin column after adsorption of phytic acid is analyzed with an analytical agent, and the 21L analytical solution is concentrated and then directly sold or hydrolyzed to produce inositol and by-products;

[0064] The analytical agent is NaCl solution, the concentration of the analytical agent is 15% wt, the dosage is 2.5 BV, and the analytical flow rate is 3 BV / h;

[0065] C: Tartaric acid was added to the effluent to adjust the pH to 1.5. Potassium reacted with tartaric acid at 20°C to form potassium hydrogen tartrate precipitate. 5350 g of crude potassium hydrogen tartrate was obtained by filtration. 100 L of the filtered filtrate was returned to the starch factory to prepare corn yellow powder.

[0066] D: Add 8 wt% dilute hydrochloric acid solution to the crude potassium hydrogen tartrate, stir and dissolve at 30°C, filter to remove the denatured protein precipitate, then add 5‰wt% activated carbon for decolorization for 1 hour, filter to obtain 17.5 L of decolorized solution, wherein the weight ratio of dilute hydrochloric acid to crude potassium hydrogen tartrate is 3:1. After drying, 365 g of the denatured protein precipitate is used as protein feed, activated carbon;

[0067] E: The decolorized liquid was neutralized to pH 2.5 by adding a 35% wt KOH solution to produce potassium hydrogen tartrate precipitate, which was centrifuged to obtain a wet product of potassium hydrogen tartrate. 17 L of the mother liquor was concentrated and potassium chloride crystals were recovered.

[0068] F: Wet potassium hydrogen tartrate was dried to obtain 2650 g of finished potassium hydrogen tartrate with a purity of 99.1% and a yield of 91.7%.

[0069] It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope limited by the appended claims of the application.

Claims

1. A process for producing potassium hydrogen tartrate using corn soaking water, characterized in that The following steps are involved: A: After the corn soaking water is allowed to settle, take the clear liquid for later use; B: The clear liquid enters the anion exchange resin column to absorb the phytic acid in the corn soaking water, and the effluent is reserved; C: Add tartaric acid to the effluent to adjust the pH to 1.5-2.

5. Potassium reacts with tartaric acid to form potassium hydrogen tartrate precipitate, which is filtered to obtain crude potassium hydrogen tartrate; D: Add dilute hydrochloric acid solution to the crude potassium hydrogen tartrate, stir to dissolve, filter to remove denatured protein precipitate, then add activated carbon for decolorization, and filter to obtain a decolorized solution; E: Add alkali to neutralize the decolorized solution to produce potassium hydrogen tartrate precipitate, which is then centrifuged and filtered to obtain the wet potassium hydrogen tartrate product; F: Wet potassium hydrogen tartrate, which is dried to obtain finished potassium hydrogen tartrate.

2. A process for producing potassium hydrogen tartrate using corn soaking water as claimed in claim 1, characterized in that: The suspended matter in step A is returned to the starch factory after sedimentation to prepare corn yellow powder.

3. A process for producing potassium hydrogen tartrate using corn soaking water as claimed in claim 1, characterized in that: The anion exchange resin column in step B is a strongly basic macroporous anion exchange resin column, with a feed volume of 8-12 BV and a feed rate of 1-3 BV / h.

4. A process for producing potassium hydrogen tartrate using corn soaking water as claimed in claim 1, characterized in that: The anion exchange resin column after adsorbing phytic acid in step B is subjected to decomposition with a decomposing agent, and the decomposition solution is concentrated and then directly sold or hydrolyzed to produce inositol and by-products; The analytical agent is one of HCl solution, KCl solution, KOH solution, NaCl solution and NaOH solution. The concentration of the analytical agent is 4-15% wt, the dosage is 1.5-2.5 BV, and the analytical flow rate is 1-3 BV / h.

5. A process for producing potassium hydrogen tartrate using corn soaking water as claimed in claim 1, characterized in that: The reaction temperature of step C is 10-20° C., and the filtrate after filtration is returned to the starch factory to prepare corn yellow powder.

6. A process for producing potassium hydrogen tartrate using corn soaking water as claimed in claim 1, characterized in that: The concentration of the dilute hydrochloric acid in step D is 5-8%wt, and the weight ratio of the added dilute hydrochloric acid to the crude potassium hydrogen tartrate is 2-3:

1.

7. A process for producing potassium hydrogen tartrate using corn soaking water as claimed in claim 1, characterized in that: The stirring temperature in step D is 30-50°C, the amount of activated carbon used is 3-5‰wt, and the decolorization time is 0.5-1h.

8. The process for producing potassium hydrogen tartrate by using corn soaking water as claimed in claim 1, wherein: The denatured protein precipitate in step D is dried and used as protein feed.

9. The process for producing potassium hydrogen tartrate by using corn soaking water as claimed in claim 1, wherein: The mother liquor from the centrifugation in step E is recycled to be used as an analytical agent after the anion exchange resin column adsorbs phytic acid in step B or to recover potassium chloride.

10. The process for producing potassium hydrogen tartrate using corn soaking water according to claim 1, wherein: The base in step E is a KOH solution with a concentration of 5-35% wt. The pH of the solution after neutralization is 1.5-2.5.