A method for improving the yield and quality of calcium citrate

Abstract

The present invention relates to the field of citrate preparation, and in particular to a method for improving the yield and quality of calcium citrate. In the calcium carbonate crushing process, calcium carbonate of different particle sizes is screened, and different calcium carbonate mass concentrations are slurried, and different combination reactions are performed according to different concentrations, and later filtering, washing and drying are performed to obtain calcium citrate, which can reduce the embedding of calcium carbonate, effectively improve the yield of calcium citrate, shorten the reaction time, reduce energy consumption, and reduce production costs.

Description

Technical Field

[0001] The invention relates to the field of citrate preparation, and in particular to a method for improving the yield and quality of calcium citrate. Background Art

[0002] Calcium citrate is widely used in human production and life. Calcium citrate can be added as a nutritional enhancer in foods such as biscuits, cakes, and bean paste; as a tissue enhancer in canned tomatoes, potatoes, etc.; as a chelating agent and buffer in the chemical industry; as an anticoagulant and artificial bone material in the medical industry; in addition, due to the high bioavailability of calcium citrate.

[0003] my country is a major producer of citric acid. At present, the world's citric acid production has reached 2 million t / a. According to statistics, my country's citric acid production capacity has reached 1.7 million t / a. The application of domestic citric acid and its downstream products is mainly concentrated in the food industry. As one of the downstream products of citric acid, calcium citrate has great market potential in animal production. However, the production method of calcium citrate is single, which has long caused the outstanding problems of high energy consumption, low yield and high cost in the preparation process of calcium citrate. Summary of the invention

[0004] In view of the problems of high energy consumption, low yield and high cost in the preparation of calcium citrate in the prior art, the present invention provides a method for improving the yield and quality of calcium citrate. The main technical scheme of the method is that in the calcium carbonate crushing step, calcium carbonate with different particle sizes is screened, and slurry with different mass concentrations of calcium carbonate is adjusted, and different combination reactions are carried out according to different concentrations, and calcium citrate is obtained by filtering, washing and drying in the later stage, which can reduce the embedding of calcium carbonate, effectively improve the yield of calcium citrate, shorten the reaction time, reduce energy consumption and reduce production cost.

[0005] The present invention provides a method for improving the yield and quality of calcium citrate, and the specific scheme is as follows:

[0006] 1) pulverizing calcium carbonate and sieving it through a sieving machine;

[0007] 2) The particles with small particle size are mixed into high-concentration calcium carbonate slurry, and the particles with large particle size are mixed into low-concentration slurry;

[0008] 3) dissolving food-grade citric acid to obtain citric acid solutions with different contents;

[0009] 4) reacting citric acid solutions from high to low with calcium carbonate slurries from high to low;

[0010] 5) When the end point pH is 4.5-5.2 and the temperature is 56-64°C, the reaction is finished;

[0011] 6) The calcium citrate after the reaction is filtered, washed, dried and packaged.

[0012] Preferably, in step 2), calcium carbonate is slurried, the mesh size of calcium carbonate particles is between 150-550 mesh, that is, the particle size is between 27-100 μm, and the slurry concentration is between 45% and 58%. Too low a concentration causes inadequate reaction, and too high a concentration causes a reaction process, increasing costs.

[0013] More preferably, the mesh number of calcium carbonate is between 150-250 mesh, and the slurry concentration is 45%-48%; the mesh number of calcium carbonate is between 250-300 mesh, and the slurry concentration is 48%-50%; the mesh number of calcium carbonate is between 300-400 mesh, and the slurry concentration is 50%-54%; the mesh number of calcium carbonate is between 400-500 mesh, and the slurry concentration is 54%-56%; the mesh number of calcium carbonate is between 500-550 mesh, and the slurry concentration is 56%-58%.

[0014] Preferably, in step 3), citric acid is dissolved and the solution content is adjusted to 6-7.3 g / 100 ml.

[0015] Preferably, in step 4), the calcium carbonate slurries with high to low concentrations are respectively added into the citric acid solutions with high to low concentrations for reaction. More preferably, the specific concentrations correspond to: the calcium carbonate slurry with a concentration of 45%-48% reacts with the citric acid solution with a content of 6.0-6.2g / 100ml; the calcium carbonate slurry with a concentration of 48%-50% reacts with the citric acid solution with a content of 6.2-6.5g / 100ml; the calcium carbonate slurry with a concentration of 50%-54% reacts with the citric acid solution with a content of 6.5-6.8g / 100ml; the calcium carbonate slurry with a concentration of 54%-56% reacts with the citric acid solution with a content of 6.8-7.0g / 100ml; the calcium carbonate slurry with a concentration of 56%-58% reacts with the citric acid solution with a content of 7.0-7.3g / 100ml.

[0016] Preferably, in step 4), the mass ratio of calcium carbonate slurry: citric acid solution is 8-10:100-110.

[0017] Carry out double decomposition reaction according to different concentrations, effectively reduce reaction time, accelerate reaction rate and improve reaction yield.

[0018] In summary, the present invention provides a method for improving the yield and quality of calcium citrate. The method comprises the following steps: screening calcium carbonate with different particle sizes in the calcium carbonate crushing step, slurrying the calcium carbonate with different particle sizes with different calcium carbonate mass concentrations, performing different combination reactions according to different concentrations, filtering, washing and drying to obtain calcium citrate in the later stage, thereby reducing the embedding of calcium carbonate, effectively improving the yield of calcium citrate, shortening the reaction time, reducing energy consumption and reducing production costs. DETAILED DESCRIPTION

[0019] The following is a further detailed description of the above contents of the present invention through specific implementation methods in the form of embodiments, but this should not be understood as the scope of the above subject matter of the present invention being limited to the following examples. All technologies implemented based on the above contents of the present invention belong to the scope of the present invention, and unless otherwise specified, the following embodiments are all completed using conventional existing technologies.

[0020] Example 1

[0021] 1) Use Muyang SKU: 5284224E5D1BC model grinder for grinding, adjust the grinding mode to the micro-grinding mode, grind the calcium carbonate, and screen it.

[0022] 2) Calcium carbonate with a mesh size of 150-250 mesh, i.e. a particle size of 60-100 μm, is slurried to a concentration of 45-48%.

[0023] 3) Dissolve citric acid and adjust the solution content to 6.0-6.2 g / 100 mL.

[0024] 4) Adding the above calcium carbonate slurry flow to the citric acid solution for reaction, wherein the mass ratio of calcium carbonate slurry to citric acid solution is 1-1.07:11.06-11.43, and the reaction ends when the end point pH is 4.5-5.2 and the temperature is 56-64°C.

[0025] Example 2

[0026] 1) Use Muyang SKU: 5284224E5D1BC model grinder for grinding, adjust the grinding mode to the micro-grinding mode, grind the calcium carbonate, and screen it.

[0027] 2) Calcium carbonate with a mesh size of 250-300 mesh, i.e. a particle size of 50-60 μm, is slurried to a concentration of 48-50%.

[0028] 3) Dissolve citric acid and adjust the solution content to 6.2-6.5 g / 100 mL.

[0029] 4) adding the above calcium carbonate slurry flow to the citric acid solution for reaction, wherein the mass ratio of calcium carbonate slurry to citric acid solution is 1-1.04:10.99-11.52, and the reaction ends when the end point pH is 4.5-5.2 and the temperature is 56-64°C.

[0030] Example 3

[0031] 1) Use Muyang SKU: 5284224E5D1BC model grinder for grinding, adjust the grinding mode to the micro-grinding mode, grind the calcium carbonate, and screen it.

[0032] 2) Calcium carbonate with a mesh size of 300-400 mesh, i.e. a particle size of 38-50 μm, is slurried to a concentration of 50%-54%.

[0033] 3) Dissolve citric acid and adjust the solution content to 6.5-6.8 g / 100 ml.

[0034] 4) Adding the above calcium carbonate slurry flow to the citric acid solution for reaction, wherein the mass ratio of calcium carbonate slurry: citric acid solution is 1-1.08:11.34-11.86, and the reaction ends when the end point pH is 4.5-5.2 and the temperature is 56-64°C.

[0035] Example 4

[0036] 1) Use Muyang SKU: 5284224E5D1BC model grinder for grinding, adjust the grinding mode to the micro-grinding mode, grind the calcium carbonate, and screen it.

[0037] 2) Calcium carbonate with a mesh size of 400-500 mesh, i.e. a particle size of 30-38 μm, is slurried to a concentration of 54%-56%.

[0038] 3) Dissolve citric acid and adjust the solution content to 6.8-7.0 g / 100 ml.

[0039] 4) adding the above calcium carbonate slurry flow to the citric acid solution for reaction, wherein the mass ratio of calcium carbonate slurry to citric acid solution is 1-1.04:11.43-11.76, and the reaction ends when the end point pH is 4.5-5.2 and the temperature is 56-64°C.

[0040] Example 5

[0041] 1) Use Muyang SKU: 5284224E5D1BC model grinder for grinding, adjust the grinding mode to the micro-grinding mode, grind the calcium carbonate, and screen it.

[0042] 2) Calcium carbonate with a mesh size of 500-550 mesh, i.e. a particle size of 27-30 μm, is slurried to a concentration of 56%-58%.

[0043] 3) Dissolve citric acid and adjust the solution content to 7.0-7.3 g / 100 ml.

[0044] 4) adding the above calcium carbonate slurry flow to the citric acid solution for reaction, wherein the mass ratio of calcium carbonate slurry to citric acid solution is 1-1.04:11.35-11.84, and the reaction ends when the end point pH is 4.5-5.2 and the temperature is 56-64°C.

[0045] Comparative Example 1

[0046] This comparative example adopts the method commonly used in the current industry:

[0047] 1) Use Muyang SKU: 5284224E5D1BC model crusher for crushing.

[0048] 2) Calcium carbonate with a mesh size of 200-250 mesh, i.e. a particle size of 60-75 μm, is slurried to a concentration of 50-55%.

[0049] 3) Dissolve citric acid and adjust the solution content to 6-8g / 100ml.

[0050] 4) Adding the above calcium carbonate slurry flow to the citric acid solution for reaction, wherein the mass ratio of calcium carbonate slurry to citric acid solution is 1-1.10:9.82-13.10, and the reaction ends when the end point pH is 4.5-5.2 and the temperature is 56-64°C.

[0051] Comparative Example 2

[0052] 1) Use Muyang SKU: 5284224E5D1BC model crusher for crushing.

[0053] 2) Calcium carbonate with a mesh size of 150-550 mesh, i.e. a particle size of 27-100 μm, is slurried to a concentration of 45-58%.

[0054] 3) Dissolve citric acid and adjust the solution content to 6.0-7.3 g / 100 ml.

[0055] 4) adding the above calcium carbonate slurry flow to the citric acid solution for reaction, wherein the mass ratio of calcium carbonate slurry to citric acid solution is 1-1.29:11.35-13.81, and the reaction ends when the end point pH is 4.5-5.2 and the temperature is 56-64°C.

[0056] The reaction raw materials of the above-mentioned embodiments and comparative examples are: 840 kg of calcium carbonate and 1200 kg of citric acid. The reaction time, calcium carbonate embedding condition, calcium citrate yield, calcium content, etc. are measured, as shown in the following table:

[0057]

[0058] From the comparison of the implementation effects in the above table, it can be seen that compared with the conventional process in the industry, the method of the present invention does not require particularly fine mesh size requirements for calcium carbonate, which reduces the difficulty of the crushing process, and takes a different approach to reduce the embedding of calcium carbonate and improve the yield of citric acid by matching the mesh size of calcium carbonate and the slurry concentration with the corresponding concentration of citric acid solution. It overcomes the shortcomings of the traditional process, improves product quality, simplifies the production process, reduces the difficulty of operation and production cost, and improves production efficiency, which is very suitable for enterprise promotion and implementation.

[0059] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any equivalent substitutions, modifications, etc. made by technicians in this field without any creative work within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for improving the yield and quality of calcium citrate, characterized in that: The specific steps include: 1) pulverizing calcium carbonate and sieving it through a sieving machine; 2) The particles with small particle size are mixed into high-concentration calcium carbonate slurry, and the particles with large particle size are mixed into low-concentration slurry; 3) dissolving food-grade citric acid to obtain citric acid solutions with different contents; 4) reacting citric acid solutions from high to low with calcium carbonate slurries from high to low; 5) When the end point pH is 4.5-5.2 and the temperature is 56-64°C, the reaction is finished; 6) filtering, washing, drying and packaging the reacted calcium citrate; In step 2), the calcium carbonate is slurried and the mesh size of the calcium carbonate particles is between 150-550 meshes, that is, the particle size is between 27-100 μm, and the slurry concentration is between 45% and 58%.

2. A method for improving the yield and quality of calcium citrate according to claim 1, characterized in that: When the mesh number of calcium carbonate is between 150-250 mesh, its slurry concentration is 45%-48%; when the mesh number of calcium carbonate is between 250-300 mesh, its slurry concentration is 48%-50%; when the mesh number of calcium carbonate is between 300-400 mesh, its slurry concentration is 50%-54%; when the mesh number of calcium carbonate is between 400-500 mesh, its slurry concentration is 54%-56%; when the mesh number of calcium carbonate is between 500-550 mesh, its slurry concentration is 56%-58%.

3. A method for improving the yield and quality of calcium citrate according to claim 1, characterized in that: In step 3), citric acid is dissolved and the solution content is adjusted to 6-7.3 g / 100 ml.

4. A method for improving the yield and quality of calcium citrate according to claim 1, characterized in that: In step 4), the calcium carbonate slurries with high to low concentrations are respectively added into the citric acid solutions with high to low concentrations for reaction, and the specific concentrations correspond to: the calcium carbonate slurry with a concentration of 45%-48% reacts with the citric acid solution with a content of 6.0-6.2g / 100ml; the calcium carbonate slurry with a concentration of 48%-50% reacts with the citric acid solution with a content of 6.2-6.5g / 100ml; the calcium carbonate slurry with a concentration of 50%-54% reacts with the citric acid solution with a content of 6.5-6.8g / 100ml; the calcium carbonate slurry with a concentration of 54%-56% reacts with the citric acid solution with a content of 6.8-7.0g / 100ml; and the calcium carbonate slurry with a concentration of 56%-58% reacts with the citric acid solution with a content of 7.0-7.3g / 100ml.

5. A method for improving the quality of calcium citrate according to claim 1, characterized in that: In step 4), the mass ratio of calcium carbonate slurry to citric acid solution is 8-10:100-110.

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