Preparation method of fructose sodium diphosphate

Abstract

The invention discloses a preparation method of fructose sodium diphosphate. The method comprises the steps that phosphate and glucose react in the presence of beer yeast subjected to freezing treatment, the freezing treatment comprises the steps that the beer yeast is placed in the environment of minus 17 DEG C to minus 14 DEG C to be frozen, and the number of freezing days is controlled to be not less than 12 days. According to the method, the beer yeast is subjected to freezing treatment and then is used for synthesizing the fructose sodium diphosphate, so that the yield of the fructose sodium diphosphate is remarkably increased, and the freezing treatment process does not generate waste liquid and is more environment-friendly.

Description

Technical Field

[0001] The present invention relates to a method for preparing sodium fructose diphosphate. Background Art

[0002] Fructose diphosphate (FDP) is an important intermediate metabolite in the process of glucose glycolysis in the body. It exists in human and all other higher animal and plant cells, and has the activity of regulating several enzymes in sugar metabolism and restoring and improving cell metabolism at the molecular level. Exogenous fructose diphosphate can act on the cell membrane, increase the concentration of high-energy phosphate bonds and adenosine triphosphate in the cell by activating phosphofructokinase on the cell membrane, thereby promoting the influx of potassium ions, restoring the cell resting state, increasing the content of diphosphoglyceric acid in red blood cells, inhibiting the release of oxygen free radicals and histamine, and being beneficial to cell energy metabolism and the utilization of glucose in states such as shock, ischemia, hypoxia, tissue damage, extracorporeal circulation, blood transfusion, etc., playing a role in promoting repair and improving cell function. In the market, its sodium salt - sodium fructose diphosphate is mostly used.

[0003] The reaction section in the production process of sodium fructose diphosphate is the first step, and the reaction process directly determines the yield of the final product. The main problem in the production process of sodium fructose diphosphate in the prior art is the low yield. In previous research, we developed a production process flow of sodium fructose diphosphate, see Patent CN102154399A for details. However, with the in-depth research, we found that although it can improve the product yield to a certain extent, the yield is still not high, and the use of toluene is not environmentally friendly.

[0004] Based on this, we need to develop a method for preparing sodium fructose diphosphate with a higher yield and more environmental friendliness. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a method for preparing sodium fructose diphosphate with a higher yield and more environmental friendliness.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] A method for preparing sodium fructose diphosphate, the preparation method includes reacting phosphate with glucose in the presence of beer yeast after freezing treatment, and the freezing treatment includes freezing the beer yeast in an environment of -17 to -14 °C, and controlling the number of days of freezing to be not less than 12 days.

[0008] Preferably, the number of days of freezing is controlled to be 12 to 18 days.

[0009] More preferably, the number of days of freezing is controlled to be 14 to 16 days.

[0010] Preferably, the brewer's yeast is waste brewer's yeast, such as the yeast discarded after beer fermentation in the beer industry.

[0011] In some embodiments, the brewer's yeast is the pressed brewer's yeast mud.

[0012] Preferably, the mass ratio of the glucose to the brewer's yeast in the feeding is 1:(0.5 - 2), more preferably 1:(0.8 - 1.3), such as 1:0.8, 1:0.9, 1:1, 1:1.1, 1:1.2, 1:1.3.

[0013] Preferably, the phosphate is sodium dihydrogen phosphate.

[0014] Preferably, the mass ratio of the phosphate to the glucose in the feeding is (0.5 - 1):1, such as 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1.

[0015] Preferably, the temperature of the reaction is controlled at 25 - 60 °C, such as 25 °C, 30 °C, 35 °C, 40 °C, 45 °C, 50 °C, 55 °C, 60 °C.

[0016] Preferably, the time of the reaction is controlled at 10 - 18 h, such as 10 h, 12 h, 14 h, 16 h, 18 h.

[0017] Preferably, the preparation method specifically includes adding pure water into a reaction tank, then adding phosphate and glucose, stirring to dissolve them, and then adding the frozen brewer's yeast for reaction.

[0018] More preferably, the mass ratio of the pure water to the glucose in the feeding is (0.05 - 0.1):1.

[0019] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:

[0020] By subjecting the brewer's yeast to freezing treatment and then using it for the synthesis of sodium fructose diphosphate, the present invention significantly improves the yield of sodium fructose diphosphate, and the freezing treatment process does not produce waste liquid, which is more environmentally friendly. Detailed Embodiments

[0021] In the production process of sodium fructose diphosphate in the prior art, there is mainly a problem of low yield. In previous research, we developed a production process flow of sodium fructose diphosphate, as detailed in Patent CN102154399A. However, with the in-depth research, we found that although it can improve the product yield to a certain extent, the yield is still not high, and the use of toluene is not environmentally friendly and also increases the treatment cost. Based on this, we developed a more environmentally friendly and higher-yield preparation method of sodium fructose diphosphate on the basis of Patent CN102154399A, which is further described below.

[0022] A preparation method of sodium fructose diphosphate, the preparation method includes reacting phosphate with glucose in the presence of beer yeast after freezing treatment, and the freezing treatment includes freezing the beer yeast in an environment of -17 to -14°C, and controlling the number of days of freezing to be not less than 12 days.

[0023] The inventors found that freezing beer yeast at -17 to -14°C for more than 12 days is more beneficial to the synthesis of sodium fructose diphosphate. The inventors speculated that under this condition, the beer yeast can be completely or substantially completely broken, thereby releasing invertase and promoting the synthesis of sodium fructose diphosphate. Compared with the method of using toluene to break the wall of beer yeast, the effect of freezing to break the wall is better, and no other reagents are introduced. On the one hand, the cost is reduced, and on the other hand, the post-treatment steps of reagent recovery are reduced, which is more environmentally friendly and has better economic benefits. The inventors also tried to use the method of repeated freezing and thawing to break the wall of beer yeast during the exploration process, but the effect was not ideal.

[0024] In the present invention, the beer yeast can be waste beer yeast (such as the beer yeast mud after pressing), and the use of waste beer yeast greatly reduces the cost, realizes the reuse of beer yeast, and has good industrial application prospects.

[0025] The present invention will be further described below in conjunction with embodiments. However, the present invention is not limited to the following embodiments. The implementation conditions adopted in the embodiments can be further adjusted according to different requirements of specific use, and the implementation conditions not specified are conventional conditions in this industry. The technical features involved in each implementation manner of the present invention can be combined with each other as long as they do not conflict with each other.

[0026] Unless otherwise specified, the raw materials involved in the following examples and comparative examples are commercially available products.

[0027] Example 1

[0028] A preparation method of sodium fructose diphosphate includes the following steps:

[0029] (1) Place the beer yeast mud after pressing at -16°C for 15 days;

[0030] (2) Add 5000 kg of pure water to the reaction tank, turn on the stirring and the jacket hot water heating, add 350 kg of sodium dihydrogen phosphate and 400 kg of glucose in sequence, stir to dissolve them, then add 400 kg of the above-treated yeast, and react at 45 - 50 °C for 14 h to obtain sodium fructose diphosphate. Measure the content of sodium fructose diphosphate in the reaction solution and calculate the yield of sodium fructose diphosphate.

[0031] In this example, the yield of sodium fructose diphosphate is 90%.

[0032] Comparative Example 1

[0033] A method for preparing sodium fructose diphosphate includes the following steps:

[0034] Add 5000 kg of pure water to the reaction tank, turn on the stirring and the jacket hot water heating, add 350 kg of sodium dihydrogen phosphate and 400 kg of glucose in sequence, stir to dissolve them, then add 400 kg of the pressed beer yeast mud, and react at 45 - 50 °C for 14 h. Measure the content of sodium fructose diphosphate in the reaction solution and calculate the yield of sodium fructose diphosphate.

[0035] In this comparative example, the yield of sodium fructose diphosphate < 10%.

[0036] By comparing Example 1 and Comparative Example 1, it is found that the pressed beer yeast mud without freezing treatment can hardly promote the synthesis of sodium fructose diphosphate, and the synthesis of sodium fructose diphosphate can be promoted by placing the beer yeast mud at -16 °C for 15 days.

[0037] Comparative Example 2

[0038] A method for preparing sodium fructose diphosphate includes the following steps:

[0039] (1) Place the pressed beer yeast mud at -16 °C for 10 days;

[0040] (2) Add 5000 kg of pure water to the reaction tank, turn on the stirring and the jacket hot water heating, add 350 kg of sodium dihydrogen phosphate and 400 kg of glucose in sequence, stir to dissolve them, then add 400 kg of the above-treated yeast, and react at 45 - 50 °C for 14 h to obtain sodium fructose diphosphate. Measure the content of sodium fructose diphosphate in the reaction solution and calculate the yield of sodium fructose diphosphate.

[0041] In this comparative example, the yield of sodium fructose diphosphate is 75%.

[0042] Comparative Example 3

[0043] (1) Place the pressed beer yeast mud at -16 °C for 5 days;

[0044] (2) Add 5000 kg of pure water to the reaction tank, start stirring and heating with hot water in the jacket. Sequentially add 350 kg of sodium dihydrogen phosphate and 400 kg of glucose, stir to dissolve them, then add 400 kg of the above-treated yeast, and react at 45 - 50 °C for 14 h to obtain sodium fructose diphosphate. Measure the content of sodium fructose diphosphate in the reaction solution and calculate the yield of sodium fructose diphosphate.

[0045] In this comparative example, the yield of sodium fructose diphosphate was 50%.

[0046] By comparing Example 1 with Comparative Examples 1 to 3, it was found that subjecting the beer yeast mud to freezing treatment could significantly increase the yield of sodium fructose diphosphate. As the number of freezing days increased, the increase in the yield of sodium fructose diphosphate became more obvious. Preferably, the number of freezing days is 12 - 18 days.

[0047] Comparative Example 4

[0048] A method for preparing sodium fructose diphosphate includes the following steps:

[0049] (1) Place the pressed beer yeast mud at -10 °C for 18 days;

[0050] (2) Add 5000 kg of pure water to the reaction tank, start stirring and heating with hot water in the jacket. Sequentially add 350 kg of sodium dihydrogen phosphate and 400 kg of glucose, stir to dissolve them, then add 400 kg of the above-treated yeast, and react at 45 - 50 °C for 14 h to obtain sodium fructose diphosphate. Measure the content of sodium fructose diphosphate in the reaction solution and calculate the yield of sodium fructose diphosphate.

[0051] In this comparative example, the yield of sodium fructose diphosphate was 62%.

[0052] Comparative Example 5

[0053] A method for preparing sodium fructose diphosphate includes the following steps:

[0054] (1) Place the pressed beer yeast mud at -25 °C for 18 days;

[0055] (2) Add 5000 kg of pure water to the reaction tank, start stirring and heating with hot water in the jacket. Sequentially add 350 kg of sodium dihydrogen phosphate and 400 kg of glucose, stir to dissolve them, then add 400 kg of the above-treated yeast, and react at 45 - 50 °C for 14 h to obtain sodium fructose diphosphate. Measure the content of sodium fructose diphosphate in the reaction solution and calculate the yield of sodium fructose diphosphate.

[0056] In this comparative example, the yield of sodium fructose diphosphate was 65%.

[0057] Comparative Example 6

[0058] A preparation method of sodium fructose diphosphate, comprising the following steps:

[0059] (1) Freeze the pressed beer yeast mud at -16°C, thaw it at room temperature, repeat three times, with a total duration of 15 days;

[0060] (2) Add 5000 kg of pure water to the reaction tank, start stirring and heating with jacket hot water, sequentially add 350 kg of sodium dihydrogen phosphate and 400 kg of glucose and stir to dissolve them, then add 400 kg of the above-treated yeast, react at 45 - 50°C for 14 h to obtain sodium fructose diphosphate. Measure the content of sodium fructose diphosphate in the reaction solution and calculate the yield of sodium fructose diphosphate.

[0061] In this comparative example, the yield of sodium fructose diphosphate is 70%.

[0062] The above has made a detailed description of the present invention, aiming to enable those skilled in this field to understand the content of the present invention and implement it. However, it cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit and essence of the present invention should be covered within the protection scope of the present invention.

Claims

1. A preparation method of sodium fructose diphosphate, characterized in that, the preparation method includes reacting phosphate with glucose in the presence of beer yeast after freezing treatment, and the freezing treatment includes freezing the beer yeast in an environment of -17 to -14 °C, and controlling the number of days of the freezing to be not less than 12 days.

2. The preparation method of sodium fructose diphosphate according to claim 1, characterized in that, controlling the number of days of the freezing to be 12 to 18 days.

3. The preparation method of sodium fructose diphosphate according to claim 1, characterized in that, the beer yeast is waste beer yeast.

4. The preparation method of sodium fructose diphosphate according to claim 3, characterized in that, the beer yeast is beer yeast mud after pressing.

5. The preparation method of sodium fructose diphosphate according to claim 1, characterized in that, the feeding mass ratio of the glucose to the beer yeast is 1:(0.5 - 2).

6. The preparation method of sodium fructose diphosphate according to claim 1, characterized in that, the phosphate is sodium dihydrogen phosphate.

7. The preparation method of sodium fructose diphosphate according to claim 1 or 6, characterized in that, the feeding mass ratio of the phosphate to the glucose is (0.5 - 1):

1.

8. The preparation method of sodium fructose diphosphate according to claim 1, characterized in that, controlling the reaction temperature to be 25 to 60 °C.

9. The preparation method of sodium fructose diphosphate according to claim 1 or 8, characterized in that, controlling the reaction time to be 10 to 18 h.

10. The preparation method of sodium fructose diphosphate according to claim 1, characterized in that, the preparation method specifically includes adding pure water into a reaction tank, then adding phosphate and glucose, stirring to dissolve them, and then adding the beer yeast after freezing treatment to react.