Preparation method of low-cost sodium phytate
By soaking in acidic aqueous solution and cleaning of circulating water, combined with acid cation exchange and alkaline treatment of the main reaction device, the problems of high cost and high pollution in the existing sodium phytate production methods are solved, and low-cost and environmentally friendly Preparation of sodium phytate, suitable for large-scale production.
Patent Information
- Application Number
- CN202411330088.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-24
- Publication Date
- 2024-12-17
AI Technical Summary
The existing sodium phytate production methods have problems of high cost and high pollution emissions, especially the high cost of raw materials, large wastewater emissions, and complex processes, making it difficult to achieve low-cost and environmentally friendly production.
A low-cost preparation method is adopted, including degreasing the plant raw materials and soaking them in an acidic aqueous solution, cleaning them by ultrasonic stirring and circulating water, using the main reaction device to perform cation exchange under acidic conditions, and processing with alkaline reaction solution. It realizes the preparation of sodium phytate, and most water resources are recycled. The process is simple and suitable for large-scale production.
It realizes low-cost and environmentally friendly preparation of sodium phytate, with simple process and high water resource utilization, suitable for large-scale production, reduces production costs and pollution emissions, and improves production efficiency and product purity.
Smart Images
Figure CN119143795A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of food additives, and in particular to a method for preparing low-cost sodium phytate. Background Art
[0002] There are currently two methods for producing sodium phytate. One is to extract phytic acid from phytin, add dilute hydrochloric acid for acid hydrolysis to obtain a mixture of phytic acid and CaCl2, and remove CaCl2 through a cation exchange resin. 2+ , a mixture of phytic acid and HCl was obtained, which was saturated with an acrylic anion resin and washed with water to remove Cl - , then add NaOH, adjust the pH, concentrate and crystallize, and dry to obtain sodium phytate. This method requires multiple ion exchanges, adsorption, and impurity removal, and the amount of wastewater discharged is large and the salt content is high. Another method is to directly neutralize phytic acid with sodium hydroxide, and then concentrate, crystallize, and dry to obtain the final phytic acid product, but this method has a high raw material cost and is therefore not competitive.
[0003] CN116102589A discloses a method for extracting sodium phytate from corn soaking liquid, which belongs to the technical field of sodium phytate extraction. The invention uses a one-step resin to adsorb phytic acid from corn soaking water, and then uses membrane separation and chromatography column to remove impurities. The inorganic and organic matter removal rate of the raw corn slurry is more than 99%, which provides a guarantee for the production of high-quality sodium phytate products in the subsequent process. The processing method reduces the wastewater discharge per ton of product by more than 60%, and the product impurity index is lower than the existing process. Membrane separation and concentration can increase the sodium phytate concentration of the feed liquid from 5% to 15%, improve the concentration efficiency and processing costs, and achieve clean and civilized production and sustainable development. Summary of the invention
[0004] To this end, the present invention provides a method for preparing sodium phytate at a low cost to solve the above problems in the prior art.
[0005] In order to achieve the above object, the present invention provides the following technical solutions: A method for preparing low-cost sodium phytate comprises the following steps: Step (a): taking 1 part of plant raw material, refining and defatting it, adding it into 2-5 parts of acidic aqueous solution with a pH of 1-4, and soaking it for 2-5 hours with ultrasonic stirring, and dehydrating it to obtain an extract A and a residue E; Step (b): washing the slag E with 2-3 parts of circulating water, adding the washing water to 1 part of the leaching solution A, stirring evenly, and then passing it into the main reaction device for treatment to obtain a by-product solution F, which is discharged, and then passing the alkaline reaction solution G into the main reaction device to obtain a treated solution B; Step (c): adjusting the pH of the treated solution B to 7.5-8.5, concentrating and filtering to obtain a precipitate C and a filtrate D, and drying the precipitate C to obtain sodium phytate.
[0006] Plant raw materials are rich in phytic acid calcium and magnesium salts. For example, the content of phytic acid calcium in rice bran can reach 10% to 11%. Phytic acid calcium and magnesium salts are closely combined with biological raw materials and are even wrapped by the cellulose of plant raw materials. During the refinement and degreasing process, the cell structure is destroyed, and phytic acid calcium and magnesium can be dissolved after soaking.
[0007] This scheme realizes cation exchange of calcium phytate solution under acidic conditions through the main reaction device. In this scheme, the circulating water mainly comes from the water vapor in the concentration process of the treatment liquid B; the cleaning slag E is mainly to elute the residual calcium and magnesium phytate to improve the recovery rate.
[0008] Preferably, in step (a), the plant raw material is rice bran; and the acidic aqueous solution is hydrochloric acid or acetic acid aqueous solution.
[0009] Preferably, in step (b), the alkaline reaction solution G is a mixed solution of 1-1.5 mol / L sodium hydroxide and 0.5-1 mol / L sodium carbonate.
[0010] Preferably, in step (c), water vapor from the concentration process enters the circulating water, and the filtrate D is introduced into the treated liquid B.
[0011] Preferably, the main reaction device comprises a main body, wherein the upper end of the main body is provided with an inlet for leachate and an inlet for reaction liquid, the bottom is provided with an outlet for treatment liquid B and an outlet for by-product, and the inside of the main body is densely arranged from top to bottom with a dispersion layer, a main reaction layer, an activated carbon layer, a base layer and a fence plate, a treatment liquid B cavity is formed between the fence plate and the outlet for treatment liquid B, a by-product cavity is formed between the fence plate and the outlet for by-product, and the product cavity is independent of the treatment liquid B cavity. The product cavity is not connected to the treatment liquid B cavity.
[0012] Preferably, the fence panel comprises a grid plate and a guardrail, the grid plate is fixed to one side of the base layer, and the guardrail is arranged below the grid plate.
[0013] Preferably, the grid plate is composed of a fixing member and a screen, and the fixing member is connected to the main body and fixed to the periphery of the screen.
[0014] The grating is mainly used to prevent the base material in the base layer from leaking out, and the guardrail acts as a valve to control the drainage direction.
[0015] Preferably, the preparation process of the main reaction layer is: immerse the large-pore alumina bricks in a saturated ferric chloride solution to fully wet them, adjust the pH to 7-8, then take them out and let them stand to drain, immerse them in a saturated ferric chloride solution again after draining, repeat 3-5 times, and obtain the main reaction layer after drying.
[0016] This process is to embed trivalent iron ions in the alumina bricks. After repeated immersion in saturated ferric chloride solution and draining, a large amount of ferric hydroxide or ferric chloride can be filled into the pores of the alumina bricks. Too high pH will generate coarse ferric hydroxide particles, which will cause clogging of the alumina bricks.
[0017] Preferably, the activated carbon preparation process of the activated carbon layer is: slag material E is dried at low temperature and mixed with sodium carbonate powder in a mass ratio of 1:0.1-0.2, and dry-grinded for 1-2 hours to obtain a mixture, and then the mixture is placed in an anaerobic environment and roasted to obtain activated carbon.
[0018] Furthermore, the temperature of the low-temperature vacuum drying is 60-80°C, and the calcination temperature is 450-650°C.
[0019] The treatment process of the main reaction device is as follows: in step (b), after the mixed solution of 2-3 parts of circulating water for washing slag E and 1 part of leachate A enters the main reaction device, it first enters the dispersion layer. The function of the dispersion layer is to make the mixed solution evenly infiltrate the main reaction layer, so that the reaction in the main reaction layer occurs evenly, and at the same time, it acts as a ballast stone to prevent the main reaction layer or the activated carbon layer from floating. Then the mixed solution enters the main reaction layer. Since the mixed solution is acidic, calcium phytate or magnesium phytate preferentially chelates with trivalent iron to generate phytic acid iron. After the reaction, the remaining soluble calcium and magnesium salts constitute the by-product solution F. Then, an alkaline reaction solution G is introduced, and the alkaline reaction solution G is preferably sodium hydroxide, and the phytic acid iron is converted into sodium phytate and ferric hydroxide. The sodium phytate solution is discharged to obtain the treated solution B. Therefore, the amount of ferric hydroxide in the main reaction layer will not change in theory. If there is outflow, it can also be attached to the activated carbon layer, which can meet the requirements of continuous production under the conditions of the main reaction device.
[0020] Compared with the prior art, the present invention achieves the following beneficial effects: The process principle of this scheme is simple, the reagents are cheap, most of the water resources are recycled in the whole process, the production efficiency is high, the cost is low, continuous production is possible, and it is suitable for large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 This is a diagram of the main reaction device provided in Example 1 of the present invention.
[0022] Figure 2 This is a cross-sectional view of the main reaction device provided in Example 1 of the present invention.
[0023] Figure 3 Schematic diagram of the fence panel provided in Example 1 of the present invention.
[0024] Figure 4 Schematic diagram of the grid provided in Example 1 of the present invention.
[0025] In the figure: 1, main body, 2, leachate inlet, 3, reaction liquid inlet, 4, treatment liquid B outlet, 5, by-product outlet, 1-1, dispersion layer, 1-2, main reaction layer, 1-3, activated carbon layer, 1-4, base layer, 1-6, fence plate, 46, treatment liquid B cavity, 56, by-product cavity, 1-6-1, fence plate, 1-6-2, grid plate, 1-6-2-1, fixing part, 1-6-2-2, screen. DETAILED DESCRIPTION
[0026] The following is a description of the implementation of the present invention by specific embodiments. People familiar with the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0027] Example 1: A method for preparing low-cost sodium phytate, comprising the following steps: Step (a): taking 1 part of rice bran, refining and defatting it, adding it into 3 parts of hydrochloric acid with a pH of 3, and soaking it for 4 hours under ultrasonic stirring, and dehydrating it to obtain an extract A and a slag E; Step (b): washing the slag E with 3 parts of circulating water, adding the washing water to 1 part of the leaching solution A, stirring evenly, and then passing the washing water into the main reaction device for treatment to obtain a by-product solution F, which is discharged, and then a mixed solution of 1 mol / L sodium hydroxide and 0.5 mol / L sodium carbonate is passed into the main reaction device to obtain a treated solution B; like Figure 1 , 2 is the main reaction device diagram, the processing process of the main reaction device is: in step (b), after the mixed liquid of 3 parts of circulating water for cleaning slag E and 1 part of leachate A enters the main body 1 of the main reaction device from the leachate inlet 2, it first contacts the dispersion layer 1-1. The function of the dispersion layer is to make the mixed liquid evenly penetrate into the main reaction layer 1-2, so that the reaction in the main reaction layer 1-2 occurs evenly, and at the same time it acts as a ballast stone to prevent the main reaction layer 1-2 or the activated carbon layer from floating. Secondly, the mixed liquid enters the main reaction layer 1-2. Since the mixed liquid is acidic, calcium phytate or magnesium phytate preferentially chelates with trivalent iron to generate phytic iron. After the reaction, calcium chloride, magnesium chloride and other by-product solution F pass through the activated carbon layer 1-3, and then through the base layer 1-4, and after passing through the 1-6 fence plate, it enters the by-product cavity 56. Combined with Figure 2, 3, 4, before entering the by-product cavity 56, solution F first passes through the grid plate 1-6-2, then the grid plate 1-6-1 opens to the by-product cavity 56 side, and finally is discharged at the treatment liquid B outlet 4, and the grid plate 1-6-1 is closed after discharge. Subsequently, the alkaline reaction liquid G is introduced into the reaction liquid inlet 3. After entering, the alkaline reaction liquid G passes through the dispersion layer 1-1, the main reaction layer 1-2, the activated carbon layer 1-3, the base layer 1-4 in sequence, passes through the grid plate 1-6-2, and the grid plate 1-6-1 opens to the treatment liquid B cavity 46, and finally the sodium phytate solution is discharged to obtain the treatment liquid B. The alkaline reaction liquid G is preferably sodium hydroxide. In the main reaction layer 1-2, phytic acid iron reacts with the alkaline reaction liquid G to generate sodium phytate and ferric hydroxide;
[0028] Step (c): adjusting the pH of the treated liquid B to 8, concentrating and filtering to obtain a precipitate C and a filtrate D, drying the precipitate C to obtain sodium phytate, the water vapor in the concentration process entering the circulating water, and the filtrate D introducing the treated liquid B; The preparation process of the main reaction layer 1-2 is as follows: immerse the large-pore alumina brick in a saturated ferric chloride solution to fully wet it, adjust the pH to 7, then take it out and let it stand to drain, and then immerse it in a saturated ferric chloride solution again after draining, repeat 5 times, and obtain the main reaction layer 1-2 after drying; The activated carbon preparation process of the activated carbon layer 1-3 is as follows: the slag E is dried at low temperature at 70°C, mixed with sodium carbonate powder in a mass ratio of 1:0.2, and dry-ground for 2 hours to obtain a mixture, and then the mixture is calcined in an anaerobic environment at 500°C to obtain activated carbon.
[0029] Example 2: A method for preparing low-cost sodium phytate, comprising the following steps: Step (a): taking 1 part of rice bran, refining and defatting it, adding it into 5 parts of hydrochloric acid with a pH of 4, and soaking it for 4 hours under ultrasonic stirring, and dehydrating it to obtain an extract A and a slag E; Step (b): washing slag E with 3 parts of circulating water, adding the washing water to 1 part of leachate A, stirring evenly, and then passing the washing water into the main reaction device for treatment to obtain a by-product solution F, which is discharged, and then passing a mixed solution of 1.5 mol / L sodium hydroxide and 0.5 mol / L sodium carbonate into the main reaction device to obtain a treated solution B; Step (c): adjusting the pH of the treated liquid B to 8, concentrating and filtering to obtain a precipitate C and a filtrate D, drying the precipitate C to obtain sodium phytate, the water vapor in the concentration process entering the circulating water, and the filtrate D introducing the treated liquid B; The preparation process of the main reaction layer 1-2 is as follows: immerse the large-pore alumina brick in a saturated ferric chloride solution to fully wet it, adjust the pH to 8, then take it out and let it stand to drain, and then immerse it in a saturated ferric chloride solution again after draining, repeat 5 times, and obtain the main reaction layer 1-2 after drying; The activated carbon preparation process of the activated carbon layer 1-3 is as follows: the slag E is dried at low temperature at 70°C, mixed with sodium carbonate powder in a mass ratio of 1:0.2, and dry-ground for 2 hours to obtain a mixture, and then the mixture is calcined in an anaerobic environment at 500°C to obtain activated carbon.
[0030] Comparative Example 1: A method for preparing sodium phytate, comprising the following steps: Step (a): taking 1 part of rice bran, refining and defatting it, adding it into 3 parts of hydrochloric acid with a pH of 3, and soaking it for 4 hours under ultrasonic stirring, and dehydrating it to obtain an extract A and a slag E; Step (b): washing the slag E with 3 parts of water, adding the washing water to 1 part of the leaching solution A, stirring evenly, and then adding the ferric chloride solution, filtering and washing after the reaction precipitation is complete, and adding a mixed solution of 1.5 mol / L sodium hydroxide and 0.5 mol / L sodium carbonate to the precipitate to obtain a treated solution B; Step (c): adjusting the pH of the treatment solution B to 8, concentrating and filtering to obtain a precipitate C.
[0031] The comparison between Examples 1-2 and Comparative Example 1 shown in this scheme is shown in Table 1.
[0032] Yield: actual weight / theoretical weight.
[0033] Table 1
[0034] It can be seen from the above table that the present embodiment 1-2 has better production advantages relative to the comparative example 1, mainly in the following aspects: 1. High production rate and high purity, which are the prerequisites for production; 2. Low water consumption, which can save production costs; 3. Few transfer times, which means that the possibility of loss and pollution in the process is small. The present embodiment only has leaching → main reaction device → concentration → drying, i.e. 3 transfers, while the comparative example is leaching → precipitation → filtration → alkali reaction → concentration → drying, i.e. 5 transfers. At the same time, more transfer times also means that more equipment support is needed, which requires more cost. Therefore, the present scheme has the characteristics of simple process principle, cheap reagent selection, recycling of most water resources in the whole process, high production efficiency, low cost, continuous production, and suitability for large-scale production relative to the prior art.
[0035] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing low-cost sodium phytate, characterized in that: The following steps are involved: Step (a): taking 1 part of plant raw material, refining and defatting it, adding it into 2-5 parts of acidic aqueous solution with a pH of 1-4, and soaking it for 2-5 hours with ultrasonic stirring, and dehydrating it to obtain an extract A and a residue E; Step (b): washing the slag E with 2-3 parts of circulating water, adding the washing water to 1 part of the leaching solution A, stirring evenly, and then passing it into the main reaction device for treatment to obtain a by-product solution F, which is discharged, and then passing the alkaline reaction solution G into the main reaction device to obtain a treated solution B; Step (c): adjusting the pH of the treated solution B to 7.5-8.5, concentrating and filtering to obtain a precipitate C and a filtrate D, and drying the precipitate C to obtain sodium phytate.
2. The method for preparing a low-cost sodium phytate according to claim 1, characterized in that: In step (a), the plant raw material is rice bran; and the acidic aqueous solution is hydrochloric acid or acetic acid aqueous solution.
3. The method for preparing a low-cost sodium phytate according to claim 1, characterized in that: In step (b), the alkaline reaction solution G is a mixed solution of 1-1.5 mol / L sodium hydroxide and 0.5-1 mol / L sodium carbonate.
4. The method for preparing a low-cost sodium phytate according to claim 1, characterized in that: In step (c), the water vapor in the concentration process enters the circulating water, and the filtrate D is introduced into the treated liquid B.
5. The method for preparing a low-cost sodium phytate according to claim 1, characterized in that: The main reaction device comprises a main body (1), wherein the upper end of the main body (1) is provided with a leachate inlet (2) and a reaction liquid inlet (3), and the bottom is provided with a treatment liquid B outlet (4) and a by-product outlet (5); the interior of the main body (1) is densely arranged from top to bottom with a dispersion layer (1-1), a main reaction layer (1-2), an activated carbon layer (1-3), a base layer (1-4) and a fence plate (1-6); a treatment liquid B cavity (46) is formed between the fence plate (1-6) and the treatment liquid B outlet (4); a by-product cavity (56) is formed between the fence plate (1-6) and the by-product outlet (5); and the product cavity (56) is independent of the treatment liquid B cavity (46).
6. The method for preparing low-cost sodium phytate according to claim 5, characterized in that: The fence plate (1-6) comprises a fence plate (1-6-2) and a fence plate (1-6-1), wherein the fence plate (1-6-2) is fixed to one side of a base layer (1-4), and the fence plate (1-6-1) is arranged below the fence plate (1-6-2).
7. The method for preparing low-cost sodium phytate according to claim 6, characterized in that: The grid plate (1-6-2) is composed of a fixing member (1-6-2-1) and a screen (1-6-2-2); the fixing member (1-6-2-1) is connected to the main body (1) and fixed to the outer periphery of the screen (1-6-2-2).
8. The method for preparing low-cost sodium phytate according to claim 5, characterized in that: The preparation process of the main reaction layer (1-2) is as follows: immersing the large-pore alumina brick in a saturated ferric chloride solution to fully wet it, adjusting the pH to 7-8, then taking it out and letting it stand to drain, and then immersing it in a saturated ferric chloride solution again after draining, repeating this process 3-5 times, and obtaining the main reaction layer (1-2) after drying.
9. The method for preparing low-cost sodium phytate according to claim 5, characterized in that: The activated carbon preparation process of the activated carbon layer (1-3) is as follows: the slag material E is dried at low temperature, mixed with sodium carbonate powder in a mass ratio of 1:0.1-0.2, and dry-ground for 1-2 hours to obtain a mixture, and then the mixture is placed in an anaerobic environment and roasted to obtain activated carbon.
10. The method for preparing low-cost sodium phytate according to claim 9, characterized in that: The temperature of the low-temperature vacuum drying is 60-80°C, and the calcination temperature is 450-650°C.