Process method for separating inositol, potassium chloride and protein by using phytine hydrolysate

Abstract

The invention relates to the technical field of inositol production, in particular to a process method for separating inositol, potassium chloride and protein by using phytine hydrolysate, which comprises the following steps: by taking phytine hydrolysate as a raw material, adding a neutralizing agent, filtering after reaction, drying a collected filter cake, treating the collected filtrate by a first hollow fiber membrane, and drying the treated filtrate by a second hollow fiber membrane; treating the collected first trapped fluid through a second hollow fiber membrane, then concentrating and decoloring the collected second trapped fluid, and cooling, crystallizing, filtering and drying the collected decolored fluid to obtain an inositol product; concentrating the collected second permeate twice, cooling, preserving heat, crystallizing, filtering and drying to obtain a potassium chloride product; and merging the collected filtrate and the first trapped fluid, concentrating, filtering, and drying to obtain the protein. According to the process method, the inositol product with high purity and high yield can be obtained, tricalcium phosphate, potassium chloride and protein products can also be obtained, and the discharge amount of waste water or waste liquid is also reduced.

Description

Technical Field

[0001] The invention relates to the technical field of inositol production, and in particular to a process for separating inositol, potassium chloride and protein by utilizing phytin hydrolyzate. Background Art

[0002] Inositol, as a natural substance beneficial to the human body, is an important vitamin required by higher animals. Inositol can promote fat metabolism and energy conversion, help regulate the water balance inside and outside cells, and maintain normal physiological functions of the body. In addition, inositol is also involved in the regulation of cholesterol and blood lipids, which helps prevent cardiovascular diseases. In terms of the nervous system, inositol has a positive effect on the health and metabolism of brain cells, and may help improve cognitive function and memory. At the same time, inositol can also enhance the effect of vitamin E, and promote the body's antioxidant defense system under synergistic effects.

[0003] The current inositol production process generally includes the processes of hydrolysis of phytin, concentration, crude crystallization, decolorization, recrystallization, centrifugation, drying, etc. However, the production process has the following defects: the soluble impurities such as potassium chloride and protein contained in phytin will interfere with the crystallization of inositol and reduce the crystallization yield. When the impurity concentration in the inositol crystallization mother liquor is too high, inositol cannot be crystallized and can only be discharged as waste liquid; the two-step crystallization method has an inositol yield of 60-70% in the recrystallization process, which is low, increases the processing cost, and there will be inositol loss during the processing.

[0004] Existing patent discloses a kind of environmentally friendly production method of inositol, comprising the following steps: after neutralizing the hydrolyzate of Phytin, filtering, cooling and filtering after the filtrate is concentrated by a multi-effect concentration system, the filtrate after cooling and filtering enters into a chromatographic separation system for separation, and collects inositol phase and salt phase; the salt phase is concentrated and crystallized to obtain a byproduct of potassium chloride; the collected inositol phase is processed by a cation exchange resin column, an anion exchange resin column, and a weakly polar macroporous adsorption resin column connected in series successively, and a pure inositol solution is obtained; after the inositol solution is concentrated by a nanofiltration membrane, a nanofiltration membrane concentrate is obtained, and the nanofiltration membrane concentrate is pumped into a multi-effect vacuum concentrator for secondary concentration treatment to obtain an inositol concentrate; after the inositol concentrate is finely filtered, it enters into a spray fluidized granulation tower for treatment to obtain an inositol finished product. This process method requires operations such as chromatographic separation and resin impurity removal, and intermediate control requirements are relatively high. The obtained products are very prone to carbonyl ammonia reaction during hot concentration, which affects product color; in addition, a large amount of waste water and resin regeneration waste liquid will be produced. Therefore, in view of the above problems, it is necessary to develop a process for separating inositol, potassium chloride and protein using phytin hydrolyzate. Summary of the invention

[0005] The technical problem to be solved by the present invention is: in view of the shortcomings of the prior art, a process method for separating inositol, potassium chloride and protein by using phytin hydrolyzate is provided, the yield and purity of inositol can be improved by using the process method, the color of the product can be ensured, potassium chloride and water-soluble protein products can be obtained, and the discharge of wastewater and waste liquid can be reduced.

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

[0007] A process for separating inositol, potassium chloride and protein using phytin hydrolyzate, comprising the following steps:

[0008] (1) taking the collected phytin hydrolyzate, adding a neutralizing agent and stirring, adjusting the pH to alkaline, controlling the reaction temperature and reaction time, filtering the liquid after the reaction, collecting the first filtrate for later use, and drying the collected first filter cake to obtain a tricalcium phosphate product;

[0009] (2) taking the first filtrate in step (1), treating it with a first hollow fiber membrane, and collecting a first permeate and a first retentate respectively;

[0010] (3) taking the first permeate in step (2), adjusting the pH to acidic, and then treating it with a second hollow fiber membrane, and collecting a second permeate and a second retentate respectively;

[0011] (4) taking the second retentate in step (3), and collecting the concentrated solution after heat concentration treatment and then entering the decolorization device, controlling the decolorization temperature and the flow rate of the concentrated solution, and the decolorized solution collected after the decolorization treatment is set aside;

[0012] (5) taking the decolorized solution in step (4), cooling, crystallizing and filtering, collecting the filter cake and drying to obtain the inositol product; combining the collected filtrate with the phytin hydrolyzate;

[0013] (6) taking the second permeate in step (3), subjecting it to a primary concentration treatment, and subjecting the collected first concentrated liquid to a secondary concentration treatment, cooling the collected second concentrated liquid, maintaining the temperature for crystallization, and filtering, and drying the collected filter cake to obtain a potassium chloride product, and the collected filtrate is used for later use;

[0014] (7) The first retentate in step (2) and the filtrate in step (6) are combined, concentrated, the collected concentrate is filtered, the collected filter cake is combined with the first filter cake in step (1), and the collected filtrate is spray-dried to obtain a protein product as a feed component.

[0015] As an improved technical solution, the neutralizing agent in step (1) is calcium oxide or calcium hydroxide, the pH is adjusted to 7.5-8.5, the reaction temperature is controlled to 30-60°C, and the reaction time is 1-3h.

[0016] As an improved technical solution, when the first hollow fiber membrane is used for treatment in step (2), the operating pressure is controlled to be 0.4-0.6Mpa, the operating temperature is 30-60°C, and the permeate is backwashed for 30-60s every 20-40min of operation, filtered to 8-10% of the original volume, and purified water with 1 / 2 the volume of the concentrated liquid is added 3-5 times before stopping the filtration; the material of the first hollow fiber membrane is polyvinylidene fluoride, and the model of the first hollow fiber membrane is NF-80~90.

[0017] As an improved technical solution, 1-2 wt % of hydrochloric acid is added in step (3) to adjust the pH to 5-6.

[0018] As an improved technical solution, when a second hollow fiber membrane is used for treatment in step (3), the operating pressure is controlled to be 0.8-1.0 MPa, the operating temperature is 35-55°C, and the solid content is concentrated to 10-20wt%. After adding 1 / 2 of the concentrated volume of purified water with the material 3-5 times, the filtration is stopped. The model of the second hollow fiber membrane is NF-95~97.

[0019] As an improved technical solution, the solid content of the concentrated liquid in step (4) is 50-60wt%, the decolorization equipment is a column with a diameter-to-height ratio of 1:3-5, the interior of the column is filled with regenerable activated carbon fiber, the decolorization temperature is controlled to be 85-90°C, and the feed flow rate of the concentrated liquid is 0.3-0.5BV / h.

[0020] As an improved technical solution, the decolorizing solution in step (5) is cooled to 25-40°C within 4-8 hours and then kept warm for crystallization.

[0021] As an improved technical solution, the first concentration treatment in step (6) is carried out by reverse osmosis membrane concentration, the temperature is controlled to be 30-60°C, the pressure is 4.5-6.0MPa, and the solid content of the first concentrated liquid is 10-20wt%; the second concentration treatment refers to thermal concentration, and the solid content of the second concentrated liquid is 50-70wt%.

[0022] As an improved technical solution, thermal concentration is used in the concentration treatment in step (7), and the solid content of the concentrated liquid is 55-65wt%.

[0023] After adopting the above technical solution, the beneficial effects of the present invention are:

[0024] The invention uses phytin hydrolyzate as a raw material, controls the temperature and time after adding a neutralizing agent, obtains an alkaline feed liquid, and then filters it. The collected filter cake is dried to obtain a tricalcium phosphate product. The collected filtrate is treated by a first hollow fiber membrane, and a first retentate and a first permeate are collected respectively. The collected first retentate is treated by a second hollow fiber membrane, and a second retentate and a second permeate are collected respectively. The collected second retentate is concentrated and decolorized, and the collected decolorized liquid is cooled, crystallized, filtered, and dried to obtain an inositol product. The collected filtrate is combined with the phytin hydrolyzate. The collected second permeate is concentrated once and concentrated twice, and then cooled, crystallized, filtered, and dried to obtain a potassium chloride product. The collected filtrate is combined with the first retentate, concentrated, and filtered again. The collected filter cake is dried, and the obtained protein is used as a feed component. The above process method is reasonably designed and easy to operate. It can obtain high-purity and high-yield inositol products, and can also obtain tricalcium phosphate, potassium chloride and protein products, avoiding waste, increasing economic benefits for the enterprise, and reducing the discharge of wastewater or waste liquid. DETAILED DESCRIPTION

[0025] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0026] Example 1

[0027] A process for separating inositol, potassium chloride and protein using phytin hydrolyzate, comprising the following steps:

[0028] (1) taking 1000 L of the collected phytin hydrolyzate (inositol concentration 81.1 g / L, potassium chloride concentration 12.5 g / L, protein content 37.8 g / L), adding a neutralizer (calcium oxide) and stirring, adjusting the pH to 7.5, controlling the reaction temperature at 30° C., and filtering the liquid after reacting for 1 hour through a plate and frame filter (filter cloth pore size 400 mesh), collecting the first filtrate 744.6 L for standby use, and collecting the first filter cake 727 kg and drying to obtain a tricalcium phosphate product;

[0029] (2) taking 744.6 L of the first filtrate in step (1), and treating it with the first hollow fiber membrane (controlling the operating pressure to 0.4 MPa, the operating temperature to 30°C, and back-flushing the permeate for 30 seconds every 20 minutes of operation, filtering to 8% of the original volume, adding purified water with 1 / 2 the volume of the concentrate three times and then stopping the filtration; the material of the first hollow fiber membrane is polyvinylidene fluoride, and the model of the first hollow fiber membrane is NF-80), and collecting 774.6 L of the first permeate and 59.6 L of the first retentate respectively;

[0030] (3) taking 774.6 L of the first permeate in step (2), adding 1 wt % hydrochloric acid to adjust the pH to 5, and then passing it through a second hollow fiber membrane treatment (controlling the operating pressure to be 0.8 MPa, the operating temperature to be 35° C., and concentrating it to a solid content of 10 wt %, adding 1 / 2 of the concentrated volume of purified water to carry the material three times, and then stopping the filtration, the model of the second hollow fiber membrane is NF-95), and collecting 1858.1 L of the second permeate and 823.7 L of the second retentate respectively;

[0031] (4) 823.7 L of the second retentate in step (3) was taken, and 130.3 L of the concentrate (solid content of 50 wt%) was collected after thermal concentration treatment and introduced into a decolorization device (a column with a diameter-to-height ratio of 1:3 and filled with regenerated activated carbon fiber, with a feed inlet at the top of the column and a discharge outlet at the bottom of the column) at a flow rate of 0.3 BV / h. The decolorization temperature was controlled at 85° C. 130.8 L of the collected decolorized liquid was set aside;

[0032] (5) 130.8 L of the decolorized solution in step (4) was taken, cooled to 25° C. within 4 h for crystallization and filtration, and 84.5 kg of the collected filter cake was dried to obtain the inositol product; 62.5 L of the collected filtrate was combined with the phytin hydrolyzate;

[0033] (6) taking 1858.1 L of the second permeate in step (3), and subjecting it to a primary concentration treatment (using reverse osmosis membrane concentration, controlling the temperature to 30° C. and the pressure to 4.5 MPa), collecting 166.7 L of the first concentrated solution with a solid content of 10 wt %, and subjecting it to a secondary concentration treatment (thermal concentration treatment), collecting 25.3 L of the second concentrated solution with a solid content of 50 wt %, cooling it to 25° C., keeping it warm for crystallization, filtering it, collecting 11.8 kg of the filter cake, and drying it to obtain a potassium chloride product, and collecting 19.8 L of the filtrate for later use;

[0034] (7) 59.6 L of the first retentate in step (2) and 19.8 L of the filtrate in step (6) are combined, and after concentration treatment (thermal concentration treatment), 47.9 L of concentrated solution with a solid content of 55 wt% is collected and filtered, and the collected filtrate is dried to obtain protein as a feed component; the collected filter cake is combined with the first filter cake in step (1).

[0035] Example 2

[0036] A process for separating inositol, potassium chloride and protein using phytin hydrolyzate, comprising the following steps:

[0037] (1) taking 1000 L of the collected phytin hydrolyzate (inositol concentration 81.1 g / L, potassium chloride concentration 12.5 g / L, protein content 37.8 g / L), adding a neutralizer (calcium hydroxide) and stirring, adjusting the pH to 7.7, controlling the reaction temperature at 60° C., and filtering the liquid after reacting for 1.5 h through a plate and frame filter (filter cloth pore size 400 mesh), collecting the first filtrate 742.7 L for standby use, and collecting the first filter cake 727.6 kg and drying to obtain a tricalcium phosphate product;

[0038] (2) taking 742.7 L of the first filtrate in step (1), and treating it with the first hollow fiber membrane (controlling the operating pressure to 0.5 MPa, the operating temperature to 60°C, and backwashing the permeate for 40 seconds every 25 minutes, filtering to 8.5% of the original volume, adding purified water with a volume of 1 / 2 of the concentrate for 4 times, and then stopping the filtration; the material of the first hollow fiber membrane is polyvinylidene fluoride, and the model of the first hollow fiber membrane is NF-90), and collecting more than 805.8 L of the first permeate and 63.1 L of the first retentate respectively;

[0039] (3) taking 805.8 L of the first permeate in step (2), adding 1.5 wt % hydrochloric acid to adjust the pH to 5.2, and then passing it through a second hollow fiber membrane treatment (controlling the operating pressure to be 0.9 MPa, the operating temperature to be 55° C., and concentrating it to a solid content of 12 wt %, adding 1 / 2 of the concentrated volume of purified water to carry the material four times, and then stopping the filtration, the model of the second hollow fiber membrane is NF-97), and collecting 1545.7 L of the second permeate and 672.7 L of the second retentate respectively;

[0040] (4) 672.7 L of the second retentate in step (3) was taken, and 122.8 L of the concentrate (solid content of 52 wt%) was collected after thermal concentration treatment and introduced into a decolorization device (a column with a diameter-to-height ratio of 1:5 and filled with regenerated activated carbon fiber, with a feed inlet at the top and a discharge outlet at the bottom) at a flow rate of 0.5 BV / h. The decolorization temperature was controlled at 90° C. 123.3 L of the decolorized liquid was collected for later use;

[0041] (5) Take 123.3 L of the decolorized solution in step (4), cool it to 30°C within 5 hours, keep it warm for crystallization, filter it, collect 85.1 kg of filter cake and dry it to obtain inositol product; collect 59.2 kg of filtrate i L was combined into the phytin hydrolyzate;

[0042] (6) taking 1545.7 L of the second permeate in step (3), and subjecting it to a primary concentration treatment (using reverse osmosis membrane concentration, controlling the temperature to 37° C. and the pressure to 4.8 MPa), collecting 137.5 L of the first concentrated liquid with a solid content of 12 wt %, and subjecting it to a secondary concentration treatment (thermal concentration treatment), collecting 23.2 L of the second concentrated liquid with a solid content of 55 wt %, cooling it to 28° C., keeping it warm for crystallization, filtering it, collecting 11.9 kg of the filter cake, and drying it to obtain a potassium chloride product, and collecting 17.6 L of the filtrate for later use;

[0043] (7) 63.1 L of the first retentate in step (2) and 17.6 L of the filtrate in step (6) are combined, and after concentration treatment (thermal concentration treatment), 43.8 L of concentrated solution with a solid content of 60 wt% is collected and filtered, and the collected filtrate is dried to obtain protein as a feed component; the collected filter cake is combined with the first filter cake in step (1).

[0044] Example 3

[0045] A process for separating inositol, potassium chloride and protein using phytin hydrolyzate, comprising the following steps:

[0046] (1) taking 1000 L of the collected phytin hydrolyzate (inositol concentration 81.1 g / L, potassium chloride concentration 12.5 g / L, protein content 37.8 g / L), adding a neutralizer (calcium hydroxide) and stirring, adjusting the pH to 8.0, controlling the reaction temperature at 45° C., and filtering the liquid after reacting for 2 h through a plate and frame filter (filter cloth pore size 400 mesh), collecting the first filtrate 739.8 L for standby use, and collecting the first filter cake 731.2 kg and drying to obtain a tricalcium phosphate product;

[0047] (2) taking 739.8 L of the first filtrate in step (1), and treating it with the first hollow fiber membrane (controlling the operating pressure to 0.6 MPa, the operating temperature to 45°C, and backwashing the permeate for 45 seconds every 30 minutes of operation, filtering to 9% of the original volume, adding purified water with a volume of 1 / 2 of the concentrate for 5 times, and then stopping the filtration; the material of the first hollow fiber membrane is polyvinylidene fluoride, and the model of the first hollow fiber membrane is NF-85), and collecting 843.7 L of the first permeate and 66.5 L of the first retentate respectively;

[0048] (3) taking 843.7 L of the first permeate in step (2), adding 1.6 wt % hydrochloric acid to adjust the pH to 5.5, and then passing it through a second hollow fiber membrane treatment (controlling the operating pressure to be 1.0 MPa, the operating temperature to be 42° C., and concentrating it to a solid content of 15 wt %, adding 1 / 2 of the concentrated volume of purified water to carry the material for 5 times, and then stopping the filtration, the model of the second hollow fiber membrane is NF-96), and collecting more than 2096.8 L of the second permeate and 542.5 L of the second retentate respectively;

[0049] (4) Take 542.5 L of the second retentate in step (3), collect 117.6 L of the concentrate (solid content is 55 wt%) after thermal concentration treatment, and then enter the decolorization equipment (a column with a diameter-to-height ratio of 1:4 and filled with regenerated activated carbon fiber, with a feed port at the top of the column and a discharge port at the bottom of the column) at a flow rate of 0.4 BV / h, control the decolorization temperature at 87°C, and collect 119.3 L of the decolorized liquid for use;

[0050] (5) 119.3 L of the decolorized solution in step (4) was taken, cooled to 32° C. within 6 h for crystallization and filtration, and 86.6 kg of the collected filter cake was dried to obtain the inositol product; 53.7 L of the collected filtrate was combined with the phytin hydrolyzate;

[0051] (6) taking 2096.8 L of the second permeate in step (3), and subjecting it to a primary concentration treatment (using reverse osmosis membrane concentration, controlling the temperature to 46° C. and the pressure to 5.2 MPa), collecting 112.5 L of a first concentrated solution with a solid content of 15 wt %, and subjecting it to a secondary concentration treatment (thermal concentration treatment), collecting 20.8 L of a second concentrated solution with a solid content of 60 wt %, cooling it to 30° C., keeping it warm for crystallization, filtering it, collecting 12.2 kg of a filter cake, and drying it to obtain a potassium chloride product, and collecting 15.2 L of a filtrate for later use;

[0052] (7) 66.5 L of the first retentate in step (2) and 15.2 L of the filtrate in step (6) are combined, and concentrated (thermal concentration), and 42.8 L of the concentrated solution with a solid content of 62 wt% is collected and filtered. The collected filtrate is dried to obtain protein as a feed component, and the collected filter cake is combined with the first filter cake in step (1).

[0053] Example 4

[0054] A process for separating inositol, potassium chloride and protein using phytin hydrolyzate, comprising the following steps:

[0055] (1) taking 1000 L of the collected phytin hydrolyzate (inositol concentration 81.1 g / L, potassium chloride concentration 12.5 g / L, protein content 37.8 g / L), adding a neutralizer (calcium oxide) and stirring, adjusting the pH to 8.2, controlling the reaction temperature at 42° C., and filtering the liquid after reacting for 2.5 hours through a plate and frame filter (filter cloth pore size 400 mesh), collecting the first filtrate 738.1 L for standby use, and collecting the first filter cake 735.5 kg and drying to obtain a tricalcium phosphate product;

[0056] (2) taking 738.1 L of the first filtrate in step (1), and treating it with the first hollow fiber membrane (controlling the operating pressure to 0.5 MPa, the operating temperature to 40°C, and every 35 min of operation, the permeate was backwashed for 53 s, filtered to 9.5% of the original volume, and the filtration was stopped after adding purified water with a volume of 1 / 2 of the concentrate for 4 times; the material of the first hollow fiber membrane was polyvinylidene fluoride, and the model of the first hollow fiber membrane was NF-90), and collecting 812.2 L of the first permeate and 70.2 L of the first retentate respectively;

[0057] (3) taking 812.2 L of the first permeate in step (2), adding 1.8 wt % hydrochloric acid to adjust the pH to 5.8, and then passing it through a second hollow fiber membrane treatment (controlling the operating pressure to be 0.9 MPa, the operating temperature to be 40° C., and concentrating it to a solid content of 18 wt %, adding 1 / 2 of the concentrated volume of purified water to carry the material for 5 times, and then stopping the filtration, the model of the second hollow fiber membrane is NF-95), and collecting 1880.5 L of the second permeate and 443.5 L of the second retentate respectively;

[0058] (4) Take 443.5 L of the second retentate in step (3), collect 112.1 L of the concentrate (solid content of 50-60 wt%) after thermal concentration treatment, and then enter the decolorization equipment (with a diameter-to-height ratio of 1:3 and a column filled with regenerated activated carbon fiber, with a feed inlet at the top of the column and a discharge outlet at the bottom of the column) at a flow rate of 0.5 BV / h, control the decolorization temperature at 98°C, and collect 112.8 L of the decolorized liquid for use;

[0059] (5) 112.8 L of the decolorized solution in step (4) was taken, cooled to 36° C. within 7 h for crystallization and filtration, and 86.8 kg of the collected filter cake was dried to obtain the inositol product; 47.4 L of the collected filtrate was combined with the phytin hydrolyzate;

[0060] (6) taking 1880.5 L of the second permeate in step (3), and subjecting it to a primary concentration treatment (using reverse osmosis membrane concentration, controlling the temperature to 60° C. and the pressure to 5.5 MPa), collecting 93.2 L of the first concentrated liquid with a solid content of 18 wt %, and subjecting it to a secondary concentration treatment (thermal concentration treatment), collecting 18.2 L of the second concentrated liquid with a solid content of 65 wt %, cooling it to 32° C., keeping it warm for crystallization, filtering it, collecting 11.9 kg of the filter cake, and drying it to obtain a potassium chloride product, and collecting 13.1 L of the filtrate for later use;

[0061] (7) 70.2 L of the first retentate in step (2) and 13.1 L of the filtrate in step (6) are combined, and after concentration treatment (thermal concentration treatment), 40.7 L of concentrated solution with a solid content of 65 wt% is collected and filtered, and the collected filtrate is dried to obtain protein as a feed component; the collected filter cake is combined with the first filter cake in step (1).

[0062] Example 5

[0063] A process for separating inositol, potassium chloride and protein using phytin hydrolyzate, comprising the following steps:

[0064] (1) taking 1000 L of the collected phytin hydrolyzate (inositol concentration 81.1 g / L, potassium chloride concentration 12.5 g / L, protein content 37.8 g / L), adding a neutralizer (calcium hydroxide) and stirring, adjusting the pH to 8.5, controlling the reaction temperature at 52° C., and filtering the liquid after reacting for 3 h through a plate and frame filter (filter cloth pore size 400 mesh), collecting the first filtrate 734.2 L for standby use, and collecting the first filter cake 741.1 kg and drying to obtain a tricalcium phosphate product;

[0065] (2) taking 734.2 L of the first filtrate in step (1), and treating it with the first hollow fiber membrane (controlling the operating pressure to 0.6 MPa, the operating temperature to 50°C, and backwashing the permeate for 60 seconds every 40 minutes of operation, filtering to 10% of the original volume, adding purified water with a volume of 1 / 2 of the concentrate for 5 times, and then stopping the filtration; the material of the first hollow fiber membrane is polyvinylidene fluoride, and the model of the first hollow fiber membrane is NF-80), and collecting 844.3 L of the first permeate and 73.4 L of the first retentate respectively;

[0066] (3) taking 844.3 L of the first permeate in step (2), adding 2.0 wt % hydrochloric acid to adjust the pH to 6, and then passing it through a second hollow fiber membrane treatment (controlling the operating pressure to be 1.0 MPa, the operating temperature to be 48° C., and concentrating it to a solid content of 20 wt %, adding 1 / 2 of the concentrated volume of purified water to carry the material for 5 times, and then stopping the filtration, the model of the second hollow fiber membrane is NF-95), and collecting 1790.7 L of the second permeate and 397.6 L of the second retentate respectively;

[0067] (4) 397.6 L of the second retentate in step (3) was taken, and 108.6 L of the concentrated liquid (solid content of 60 wt%) was collected after thermal concentration treatment, and the concentrated liquid was introduced into a decolorization device (a column with a diameter-to-height ratio of 1:3 and filled with regenerated activated carbon fiber, with a discharge port at the top of the column and a discharge port at the bottom of the column) at a flow rate of 0.3 BV / h, and the decolorization temperature was controlled at 90° C. 108.7 L of the collected decolorized liquid was set aside;

[0068] (5) 108.7 L of the decolorized solution in step (4) was taken, cooled to 40° C. within 8 h for crystallization and filtration, and 87.4 kg of the collected filter cake was dried to obtain the inositol product; 40.4 L of the collected filtrate was combined with the phytin hydrolyzate;

[0069] (6) taking 1790.7 L of the second permeate in step (3), and subjecting it to a primary concentration treatment (using reverse osmosis membrane concentration, controlling the temperature to 60° C. and the pressure to 4.5 MPa), collecting 83.7 L of a first concentrated solution with a solid content of 20 wt %, and subjecting it to a secondary concentration treatment (thermal concentration treatment), collecting 16.8 L of a second concentrated solution with a solid content of 70 wt %, cooling it to 35° C., keeping it warm for crystallization, filtering it, collecting 11.7 kg of filter cake, and drying it to obtain potassium chloride as potassium chloride, and collecting 10.6 L of filtrate for later use;

[0070] (7) 73.4 L of the first retentate in step (2) and 10.6 L of the filtrate in step (6) are combined, and after concentration treatment (thermal concentration treatment), 45.5 L of concentrated solution with a solid content of 58 wt% is collected, filtered, and the collected filtrate is dried to obtain protein as a feed component; the collected filter cake is combined with the first filter cake in step (1).

[0071] In order to better demonstrate that the process of the present invention can obtain high-purity and high-yield inositol products, and can also obtain high-yield tricalcium phosphate products, potassium chloride and protein products, 17 comparative examples are given with reference to Example 3, and the details are shown below.

[0072] Comparative Example 1

[0073] The difference from Example 3 is that the reaction temperature in step (1) is controlled to be 25° C., and the other operations are the same.

[0074] Comparative Example 2

[0075] The difference from Example 3 is that step (2) is missing, and the remaining operations are the same.

[0076] Comparative Example 3

[0077] The difference from Example 3 is that in step (2), the operating pressure is controlled to be 0.3 MPa, and the rest of the operations are the same.

[0078] Comparative Example 4

[0079] The difference from Example 3 is that the operating temperature of the membrane in step (2) is 20°C, and the rest of the operations are the same.

[0080] Comparative Example 5

[0081] The difference from Example 3 is that the operating temperature of the membrane in step (2) is 70° C., and the rest of the operations are the same.

[0082] Comparative Example 6

[0083] The difference from Example 3 is that the model of the membrane in step (2) is NF-75, and the rest of the operations are the same.

[0084] Comparative Example 7

[0085] The difference from Example 3 is that the model of the membrane in step (2) is NF-92, and the rest of the operations are the same.

[0086] Comparative Example 8

[0087] The difference from Example 3 is that step (3) is missing, and the remaining operations are the same.

[0088] Comparative Example 9

[0089] The difference from Example 3 is that in step (3), the operating pressure is controlled to be 0.7 MPa, and the rest of the operations are the same.

[0090] Comparative Example 10

[0091] The difference from Example 3 is that the operating temperature of the membrane in step (3) is 25°C, and the rest of the operations are the same.

[0092] Comparative Example 11

[0093] The difference from Example 3 is that the operating temperature of the membrane in step (3) is 65°C, and the rest of the operations are the same.

[0094] Comparative Example 12

[0095] The difference from Example 3 is that the model of the membrane in step (3) is NF-92, and the rest of the operations are the same.

[0096] Comparative Example 13

[0097] The difference from Example 3 is that the model of the membrane in step (3) is NF-99, and the rest of the operations are the same.

[0098] Comparative Example 14

[0099] The difference from Example 3 is that the temperature is lowered to 20° C. in step (5), and the remaining operations are the same.

[0100] Comparative Example 15

[0101] The difference from Example 3 is that the temperature is lowered to 45° C. in step (5), and the remaining operations are the same.

[0102] Comparative Example 16

[0103] The difference from Example 3 is that the temperature is lowered to 20° C. in step (6), and the remaining operations are the same.

[0104] Comparative Example 17

[0105] The difference from Example 3 is that the temperature is lowered to 38° C. in step (6), and the remaining operations are the same.

[0106] Table 1

[0107]

[0108]

[0109] It can be found from the data in Table 1 that, by adopting the process method of the present invention, compared with Example 3 and other examples and Comparative Examples 1-17, the yield, yield and purity of inositol and protein, the yield of tricalcium phosphate and the yield and purity of potassium chloride obtained are optimal.

[0110] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate, characterized in that: The following steps are involved: (1) taking the collected phytin hydrolyzate, adding a neutralizing agent and stirring, adjusting the pH to alkaline, controlling the reaction temperature and reaction time, filtering the liquid after the reaction, collecting the first filtrate for later use, and drying the collected first filter cake to obtain a tricalcium phosphate product; (2) taking the first filtrate in step (1), treating it with a first hollow fiber membrane, and collecting a first permeate and a first retentate respectively; (3) taking the first permeate in step (2), adjusting the pH to acidic, and then treating it with a second hollow fiber membrane, and collecting a second permeate and a second retentate respectively; (4) taking the second retentate in step (3), and collecting the concentrated solution after heat concentration treatment and then entering the decolorization device, controlling the decolorization temperature and the flow rate of the concentrated solution, and the decolorized solution collected after the decolorization treatment is set aside; (5) taking the decolorized solution in step (4), cooling, crystallizing and filtering, collecting the filter cake and drying to obtain the inositol product; combining the collected filtrate with the phytin hydrolyzate; (6) taking the second permeate in step (3), subjecting it to a primary concentration treatment, and subjecting the collected first concentrated liquid to a secondary concentration treatment, cooling the collected second concentrated liquid, maintaining the temperature for crystallization, and filtering, and drying the collected filter cake to obtain a potassium chloride product, and the collected filtrate is used for later use; (7) The first retentate in step (2) and the filtrate in step (6) are combined, concentrated, the collected concentrate is filtered, the collected filter cake is combined with the first filter cake in step (1), and the collected filtrate is spray-dried to obtain a protein product as a feed component.

2. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: The neutralizing agent in step (1) is calcium oxide or calcium hydroxide, the pH is adjusted to 7.5-8.5, the reaction temperature is controlled to 30-60° C., and the reaction time is 1-3 h.

3. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: When the first hollow fiber membrane is used for treatment in step (2), the operating pressure is controlled to be 0.4-0.6Mpa, the operating temperature is 30-60°C, and the permeate is backwashed for 30-60s every 20-40min of operation, filtered to 8-10% of the original volume, and purified water with 1 / 2 the volume of the concentrated liquid is added 3-5 times before stopping the filtration; the material of the first hollow fiber membrane is polyvinylidene fluoride, and the model of the first hollow fiber membrane is NF-80~90.

4. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: In step (3), 1-2 wt % hydrochloric acid is added to adjust the pH to 5-6.

5. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: When the second hollow fiber membrane is used for treatment in step (3), the operating pressure is controlled to be 0.8-1.0 MPa, the operating temperature is 35-55°C, and the solid content is concentrated to 10-20wt%. After adding 1 / 2 of the concentrated volume of purified water with the material 3-5 times, the filtration is stopped. The model of the second hollow fiber membrane is NF-95~97.

6. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: The solid content of the concentrated solution in step (4) is 50-60wt%, the decolorization equipment is a column with a diameter-to-height ratio of 1:3-5, the interior of the column is filled with regenerable activated carbon fiber, the decolorization temperature is controlled to be 85-90°C, and the feed flow rate of the concentrated solution is 0.3-0.5BV / h.

7. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: The decolorizing solution in step (5) is cooled to 25-40° C. within 4-8 hours and then kept warm for crystallization.

8. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: In step (6), the first concentration treatment is carried out by reverse osmosis membrane concentration, the temperature is controlled at 30-60°C, the pressure is 4.5-6.0MPa, and the solid content of the first concentrated liquid is 10-20wt%; the second concentration treatment refers to thermal concentration, and the solid content of the second concentrated liquid is 50-70wt%.

9. A process for separating inositol, potassium chloride and protein using phytin hydrolyzate according to claim 1, characterized in that: In step (7), thermal concentration is used for the concentration treatment, and the solid content of the concentrated solution is 55-65wt%.

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