阅读说明：本技术 一种葡萄糖酸钙-葡萄糖酸复合粉的制备方法 (Preparation method of calcium gluconate-gluconic acid composite powder ) 是由 马仕敏 李世玉 陈祥峰 于 2021-09-09 设计创作，主要内容包括：本发明涉及一种葡萄糖酸钙-葡萄糖酸复合粉的制备方法,属于食品添加剂的技术领域。本发明以葡萄糖酸钙作为吸附剂,在一定条件下,吸附高浓度的葡萄糖酸,以此来制备葡萄糖酸钙-葡萄糖酸复合粉。本发明的葡萄糖酸钙-葡萄糖酸复合粉具有溶解速度快、生物利用率高、口感好等优点,广泛应用于乳制品、饮料、食品保健品、糖果、烘焙制品等食品行业,特别是食品保鲜、防腐、改善口感、屏蔽不良气味的技术领域,同时可以螯合金属离子,具有缓慢释放的功能；并且增加葡萄糖酸钙的应用范围,弥补了葡萄糖酸钙不具备抑菌功能的缺点。(The invention relates to a preparation method of calcium gluconate-gluconic acid composite powder, belonging to the technical field of food additives. The invention takes calcium gluconate as an adsorbent, and adsorbs high-concentration gluconic acid under certain conditions to prepare the calcium gluconate-gluconic acid composite powder. The calcium gluconate-gluconic acid composite powder has the advantages of high dissolution speed, high bioavailability, good mouthfeel and the like, is widely applied to food industries such as dairy products, beverages, food health products, candies, baked products and the like, particularly the technical fields of food preservation, corrosion prevention, mouthfeel improvement and bad smell shielding, can chelate metal ions, and has a slow release function; and the application range of the calcium gluconate is enlarged, and the defect that the calcium gluconate does not have the bacteriostatic function is overcome.)

1. A preparation method of calcium gluconate-gluconic acid composite powder is characterized by comprising the following steps:

(1) crushing the anhydrous calcium gluconate, sieving with a 100-300-mesh sieve, feeding oversize products into a crusher for crushing again, and metering undersize products;

(2) concentrating gluconic acid to the mass concentration of 88-92%, transferring the gluconic acid to a reaction tank, and heating the gluconic acid to 85-90 ℃;

(3) uniformly and equivalently adding the metered undersize anhydrous calcium gluconate into a reaction tank according to 2-5 times, and uniformly stirring;

(4) after the anhydrous calcium gluconate powder is fully mixed, adding silicon dioxide into the reaction tank, and stirring at a constant speed for 60-120 min;

(5) drying the mixed material in the step (4) in a fluidized bed;

(6) and (4) cooling the dried material obtained in the step (5), and then crushing at a low temperature to obtain the calcium gluconate-gluconic acid composite powder with the crushing granularity of 60-200 meshes.

2. The method for preparing the calcium gluconate-gluconic acid composite powder of claim 1, wherein the calcium gluconate-gluconic acid composite powder comprises the following components in percentage by weight: 55-65% of gluconic acid with the mass concentration of 88-92%, 40-30% of anhydrous calcium gluconate and 2-10% of silicon dioxide.

3. The method for preparing the calcium gluconate-gluconic acid composite powder of claim 1, wherein the calcium gluconate-gluconic acid composite powder comprises the following components in percentage by weight: 60% of gluconic acid with the mass concentration of 88-92%, 35% of anhydrous calcium gluconate and 5% of silicon dioxide.

4. The method for preparing a calcium gluconate-gluconic acid composite powder according to claim 1, wherein the silicon dioxide is fumed silica.

5. The preparation method of the calcium gluconate-gluconic acid composite powder according to claim 1, wherein the step (3) adopts ribbon stirring, and the stirring speed is 30-60 rpm; stirring and mixing time is 60-120 min.

6. The preparation method of the calcium gluconate-gluconic acid composite powder according to claim 1, wherein in the step (5), the air inlet temperature of the fluidized bed is 145-160 ℃, the bed layer temperature of the fluidized bed is 85-95 ℃, the drying time is 15min, and the air exhaust temperature is 75-85 ℃.

7. The preparation method of the calcium gluconate-gluconic acid composite powder according to claim 1, wherein the step (6) adopts a low-temperature pulverizer to pulverize, and the pulverizing particle size is 60-200 meshes; and screening by using a grading sieve, wherein the grading is 60-120 meshes and 120-200 meshes.

8. The method for preparing calcium gluconate-gluconic acid composite powder according to claim 1, wherein in the step (6), the material with the granularity of more than 200 meshes after being crushed and sieved is mixed with the next batch of material.

Technical Field

The invention belongs to the technical field of food additives, and particularly relates to a preparation method of calcium gluconate-gluconic acid composite powder.

Background

Gluconolactone is used as a coagulant, a stabilizer, an acidulant, an antistaling agent and a preservative in the food industry, is a multifunctional food additive, is mainly applied to the preparation of lactone bean curd, and can generate a large amount of gluconic acid in the process of producing the gluconolactone. The gluconic acid is an organic acid, has the functions of mild mouthfeel, improving the taste of food and shielding unpleasant odor, is also an only bifidobacterium (probiotic) proliferation factor in the organic acid, can preserve other active ingredients in the food, can be slowly released, reduces the pH value of the food, extends the acidification effect to small intestines, enhances the acidification effect, improves the micro-ecological environment of the stomach and the intestinal tract, promotes the growth of probiotics, inhibits the growth of mixed bacteria and is beneficial to health.

The existing preparation method of calcium gluconate is a crystallization method, the crystallized calcium gluconate is subjected to solid-liquid separation, then is dried and crushed to obtain calcium gluconate powder, the mother liquor is subjected to biochemical treatment, the purity of the produced calcium gluconate is more than 98%, the pH value is about 7.5, and the calcium gluconate is mainly used for food reinforced calcium supplement and is mainly applied to oral administration and injection in the aspect of medicine. The water solution has poor solubility and slow dissolution speed, so the application range of the water solution in the food industry is narrow. The pH value of the food is about 7.5, so that the food does not improve the taste of the food, shield bad smell and simultaneously have no bacteriostatic function, the food is easy to deteriorate when the food is added, and the shelf life of the product is not improved.

Disclosure of Invention

Aiming at the problems of poor solubility, slow dissolution speed, no bacteriostatic function and the like of products produced in the prior art, the invention provides a preparation method of calcium gluconate-gluconic acid composite powder, which aims to solve the technical problems. The invention takes calcium gluconate as an adsorbent, and adsorbs high-concentration gluconic acid under certain conditions to prepare the calcium gluconate-gluconic acid composite powder. The calcium gluconate-gluconic acid composite powder produced by the invention solves the problems of difficult utilization, low added value, difficult transportation, high packaging cost and inconvenient use by consumers of a large amount of gluconic acid mother liquor generated in the production process of glucolactone.

The technical scheme of the invention is as follows:

a preparation method of calcium gluconate-gluconic acid composite powder comprises the following steps:

(1) crushing the anhydrous calcium gluconate, sieving with a 100-300-mesh sieve, feeding oversize products into a crusher for crushing again, and metering undersize products;

(2) concentrating gluconic acid to the mass concentration of 88-92%, transferring the gluconic acid to a reaction tank, and heating the gluconic acid to 85-90 ℃;

(3) uniformly and equivalently adding the metered undersize anhydrous calcium gluconate into a reaction tank according to 2-5 times, and uniformly stirring;

(4) after the anhydrous calcium gluconate powder is fully mixed, adding silicon dioxide into the reaction tank, and stirring at a constant speed for 60-120 min;

(5) drying the mixed material in the step (4) in a fluidized bed;

(6) and (4) cooling the dried material obtained in the step (5), and then crushing at a low temperature, wherein the crushing granularity is 60-200 meshes, so as to obtain the food-grade calcium gluconate-gluconic acid composite powder.

Preferably, the calcium gluconate-gluconic acid composite powder consists of the following components in percentage by weight: 55-65% of gluconic acid with the mass concentration of 88-92%, 40-30% of anhydrous calcium gluconate and 2-10% of silicon dioxide.

Preferably, the calcium gluconate-gluconic acid composite powder consists of the following components in percentage by weight: 60% of gluconic acid with the mass concentration of 88-92%, 35% of anhydrous calcium gluconate and 5% of silicon dioxide.

Preferably, the silica is fumed silica. The fumed silica is added to absorb partial water, so that the moisture absorption of the product is prevented, and the flowability of the product is increased.

Preferably, the step (3) adopts a helical ribbon type stirring, the stirring speed is 30-60 revolutions per minute, preferably 35 revolutions per minute, and the stirring and mixing time is 60-120 min, preferably 120 min.

Preferably, in the step (5), the air inlet temperature of the fluidized bed is 145-160 ℃, the bed layer temperature of the fluidized bed is 85-95 ℃, the drying time is 15min, and the air exhaust temperature is 75-85 ℃.

Preferably, the step (6) adopts a low-temperature pulverizer to pulverize, and the pulverizing particle size is 60-200 meshes; and screening by using a grading sieve, wherein the grading is 60-120 meshes and 120-200 meshes.

Preferably, in the step (6), the materials with the particle size of more than 200 meshes after crushing and screening are mixed with the next batch of materials. The invention has the beneficial effects that:

(1) the calcium gluconate-gluconic acid composite powder produced by the invention adsorbs more than 50% of gluconic acid by the calcium gluconate powder, so that the solubility of the calcium gluconate is increased, the pH value of the food is adjusted, the mouthfeel is improved, the antibacterial function is increased, the shelf life of the food is prolonged, and the defect that the calcium gluconate is added into the food is overcome. The calcium gluconate-gluconic acid composite powder has the advantages of high dissolution speed, high bioavailability, good mouthfeel and the like, is widely applied to food industries such as dairy products, beverages, food health products, candies, baked products and the like, particularly the technical fields of food preservation, corrosion prevention, mouthfeel improvement and bad smell shielding, can chelate metal ions, and has a slow release function.

(2) The calcium gluconate-gluconic acid composite powder produced by the invention solves the problems of difficult utilization, low additional value, difficult transportation, high packaging cost, inconvenient use by consumers and the like of a large amount of gluconic acid mother liquor generated in the production process of glucolactone. The calcium gluconate-gluconic acid composite powder produced by the invention has larger fluidity and can be well and fully mixed with other food raw materials.

(3) The calcium gluconate-gluconic acid composite powder produced by the invention increases the application range of the calcium gluconate, makes up for the defect that the calcium gluconate does not have the bacteriostatic function, and extends the application range of the calcium gluconate.

Detailed Description

In order to make those skilled in the art better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

(1) 3.6 tons of anhydrous calcium gluconate are crushed and sieved by a 200-mesh sieve, and oversize products enter a crusher to be crushed again to obtain 3.5 tons of undersize products;

(2) concentrating 12.26 tons of gluconic acid with the concentration of 52 percent to the concentration of 90 percent and the mass of 6.94 tons, then transferring the gluconic acid into a reaction tank, and heating the gluconic acid to 90 ℃;

(3) adding 3.5 tons of undersize anhydrous calcium gluconate into the reaction tank uniformly and equivalently according to 3 times, and stirring by adopting a helical ribbon type at the stirring speed of 35 revolutions per minute for 120 min;

(4) after the anhydrous calcium gluconate powder is fully mixed, adding 250kg of fumed silica into the reaction tank, and stirring at constant speed for 120 min;

(5) drying the mixed material obtained in the step (4) in a fluidized bed, wherein the air inlet temperature of the fluidized bed is 145 ℃, the bed temperature of the fluidized bed is 85-95 ℃, the drying time is 15min, and the air exhaust temperature is 75-85 ℃;

(6) and (3) cooling the dried material obtained in the step (5), crushing by using a low-temperature crusher, and screening by using a classifying screen to obtain food-grade calcium gluconate-gluconic acid composite powder, wherein the weight of the food-grade calcium gluconate-gluconic acid composite powder is 4.62 tons in 60-120 meshes, 4.78 tons in 120-200 meshes, and 0.61 ton above 200 meshes.

Example 2

(1) Crushing 4.08 tons of anhydrous calcium gluconate, sieving with a 200-mesh sieve, and crushing oversize products in a crusher again to obtain 4 tons of undersize products;

(2) concentrating 12.07 ton 50% gluconic acid to 90% concentration, 6.57 ton, transferring to a reaction tank, and heating to 85 deg.C;

(3) adding 4 tons of undersize anhydrous calcium gluconate into the reaction tank uniformly and equivalently according to 2 times, and stirring by adopting a helical ribbon type at the stirring speed of 35 revolutions per minute for 90 min;

(4) after the anhydrous calcium gluconate powder is fully mixed, adding 200kg of fumed silica into the reaction tank, and stirring at constant speed for 120 min;

(5) drying the mixed material obtained in the step (4) in a fluidized bed, wherein the air inlet temperature of the fluidized bed is 145 ℃, the bed temperature of the fluidized bed is 85-95 ℃, the drying time is 15min, and the air exhaust temperature is 75-85 ℃;

(6) and (3) cooling the dried material in the step (5), crushing by using a low-temperature crusher, and screening by using a classifying screen to obtain food-grade calcium gluconate-gluconic acid composite powder, wherein the weight of the food-grade calcium gluconate-gluconic acid composite powder is 5.54 tons in 60-120 meshes, 4.15 tons in 120-200 meshes, and 0.31 ton above 200 meshes.

Example 3

(1) Crushing 33.67 tons of anhydrous calcium gluconate, sieving with a 200-mesh sieve, and crushing oversize products in a crusher again to obtain 33 tons of undersize products;

(2) concentrating 129.2 tons of gluconic acid with the concentration of 50% to the concentration of 90%, transferring the gluconic acid to a reaction tank, and heating the gluconic acid to 90 ℃;

(3) adding 33 tons of undersize anhydrous calcium gluconate into the reaction tank uniformly and equivalently according to 5 times, and stirring by adopting a helical ribbon type at the stirring speed of 40 revolutions per minute for 90 min;

(4) after the anhydrous calcium gluconate powder is fully mixed, 5100kg of fumed silica is added into the reaction tank, and the mixture is stirred at a constant speed for 90 min;

(5) drying the mixed material obtained in the step (4) in a fluidized bed, wherein the air inlet temperature of the fluidized bed is 145 ℃, the bed temperature of the fluidized bed is 85-95 ℃, the drying time is 15min, and the air exhaust temperature is 75-85 ℃;

(6) and (3) cooling the dried material in the step (5), crushing by using a low-temperature crusher, and screening by using a classifying screen to obtain food-grade calcium gluconate-gluconic acid composite powder, wherein the weight of the food-grade calcium gluconate-gluconic acid composite powder is 63.85 tons in a 60-120 mesh, 33.75 tons in a 120-200 mesh, and 2.4 tons in a 200-mesh range.

Test example

1. The calcium gluconate-gluconic acid composite powder prepared in the embodiment 1-3 is tested, and the detection results are shown in the following table 1:

TABLE 1 results of the measurements

2. The calcium gluconate-gluconic acid composite powder prepared in example 1 and calcium gluconate are used for bread bacteriostasis comparative test. The test method is as follows:

the total number of colonies is detected according to GB4789.2-2016, the total number of colonies is detected according to GB 4789.15-2016, and the total number of Escherichia coli colonies is detected according to GB 4789.3-2016. The detection results are shown in the following tables 2-4:

TABLE 2 Total colony count

Day 0

5 days

10 days

15 days

20 days

30 days

Calcium gluconate

Is free of

Is free of

1 is provided with

3 are provided with

10 are provided with

30 pieces of

Example 1

Is free of

Is free of

Is free of

1

1

2

TABLE 3 Total number of colonies of the mold

Day 0

5 days

10 days

15 days

20 days

30 days

Calcium gluconate

Is free of

Is free of

Is free of

Is free of

1 is provided with

3 are provided with

Example 1

Is free of

Is free of

Is free of

Is free of

Is free of

Is free of

TABLE 4 Total E.coli colonies

Day 0

5 days

10 days

15 days

20 days

30 days

Calcium gluconate

Is free of

Is free of

Is free of

Is free of

Is free of

Is free of

Example 1

Is free of

Is free of

Is free of

Is free of

Is free of

Is free of

3. Solubility in water

We know that the solubility of calcium gluconate is 3.3%, so we chose to use 2%, 4%, 10% concentration for solubility comparison at room temperature, as shown in table 5 below:

TABLE 5 solubility test results

4. Dissolution rate

1g, 2g and 3g of calcium gluconate samples are put into 100ml of water with the temperature of 30 ℃, the mixture is kept still after an oscillator is used for 10s, the clarifying time of the solution is recorded, and the dissolution speed of the calcium gluconate-gluconic acid composite powder is determined according to the method in the same way, and the method is specifically as shown in the following table 6:

TABLE 6 dissolution Rate test results

Although the present invention has been described in detail by way of preferred embodiments, the present invention is not limited thereto. Various equivalent modifications or substitutions can be made on the embodiments of the present invention by those skilled in the art without departing from the spirit and scope of the present invention, and these modifications or substitutions are within the scope of the present invention/any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.