阅读说明：本技术 一种药用氯化钙生产过程中加酸工艺的控制参数确定方法 (Method for determining control parameters of acid adding process in production process of medicinal calcium chloride ) 是由 魏炳举 刘素芹 郑井瑞 王丹 张嫱嫱 于 2020-04-07 设计创作，主要内容包括：本发明公开了一种药用氯化钙生产过程中加酸工艺的控制参数确定方法,涉及药用氯化钙的生产工艺,具体涉及药用氯化钙生产过程中加酸工艺技术控制参数的确定。通过对蒸发终止温度、蒸发加酸量、干燥温度、干燥时间等工艺控制点进行试验研究,从而确定药用氯化钙生产最佳的加酸控制参数。通过该确定的工艺参数进行生产,避免了生产过程中加酸量过多对生产装置造成的腐蚀等影响,以及蒸发温度、时间等指标控制不当对生产效率及产品质量的影响,进而提高了生产效率和产品纯度。(The invention discloses a method for determining control parameters of an acid adding process in the production process of medicinal calcium chloride, relates to the production process of medicinal calcium chloride, and particularly relates to determination of control parameters of the acid adding process technology in the production process of medicinal calcium chloride. The optimal acidification control parameters for the production of the medicinal calcium chloride are determined by experimental research on process control points such as evaporation termination temperature, evaporation acidification amount, drying temperature, drying time and the like. The production is carried out by the determined process parameters, so that the influences of corrosion and the like on a production device caused by excessive acid addition in the production process and the influences of improper control of indexes such as evaporation temperature, time and the like on the production efficiency and the product quality are avoided, and the production efficiency and the product purity are further improved.)

1. A method for determining control parameters of an acid adding process in the production process of medicinal calcium chloride is characterized by comprising the following steps:

step of determining the end temperature of evaporation

Heating and evaporating a certain amount of refined calcium chloride solution to different temperature end points, drying the evaporated solution after flaking, and detecting the purity and the pH value of the product;

step of determining the amount of acid added by evaporation

Heating and evaporating a certain amount of refined calcium chloride solution, adding acid in stages in the evaporation process, controlling the acid adding amount in different stages, controlling the pH value of the evaporated solution to be 3-5, and then, testing the product purity and the pH value of the evaporated solution after flaking and drying;

step of determination of drying temperature

Heating and evaporating a certain amount of refined calcium chloride solution, cooling and tabletting an evaporated solution, drying, and checking the purity and the pH value of a product according to control of different drying temperatures;

step of determination of drying time

Heating and evaporating a certain amount of refined calcium chloride solution, cooling the evaporated solution for flaking, drying, and inspecting the purity and the pH value of the product according to different drying times.

2. The method for determining the control parameter of the acid adding process in the production process of the medicinal calcium chloride according to claim 1, which is characterized in that: the evaporation termination temperature is controlled between 155 ℃ and 175 ℃.

3. The method for determining the control parameter of the acid adding process in the production process of the medicinal calcium chloride according to claim 1, which is characterized in that: the acid adding amount of the evaporated calcium chloride solution is controlled to be 0.2-0.8% of the volume ratio of the volume of the raw material solution.

4. The method for determining the control parameter of the acid adding process in the production process of the medicinal calcium chloride according to claim 1, which is characterized in that: the drying temperature is controlled between 180 and 200 ℃.

5. The method for determining the control parameter of the acid adding process in the production process of the medicinal calcium chloride according to claim 1, which is characterized in that: the drying time is controlled to be 3-10 minutes.

6. The method for determining the control parameter of the acid adding process in the production process of the medicinal calcium chloride according to claim 1, which is characterized in that: the refined calcium chloride solution is W_CaCl2＝40～60％。

Technical Field

The invention relates to a production process of medicinal calcium chloride, in particular to determination of technical control parameters of an acid adding process in the production process of the medicinal calcium chloride.

Background

The medicinal calcium chloride is used as a chemical raw material medicine, is generally used as an electrolyte balance regulating medicine and is used for preparing calcium chloride solution, osmotic pressure regulator and the like. It is now widely used as a major component of concentrates for hemodialysis and related treatments.

At present, the production process of domestic medicinal calcium chloride is basically that industrial calcium carbonate reacts with hydrochloric acid, reaction liquid is prepared by the processes of impurity removal, evaporation, stir-frying block making, crushing and mixing and the like, acid is added in the evaporation process respectively at the early stage, the middle stage and the later stage of evaporation to adjust the pH value of a product, the control point of the acid adding process and the acid adding amount are always estimated according to experience, the existing acid adding process is likely to have excessive acid adding amount, the corrosion degree of equipment is increased, and unnecessary waste is caused. Therefore, the experiment is an experimental study on how much acid is added in the evaporation process.

Disclosure of Invention

The invention aims to provide a method for determining control parameters of an acid adding process in the production process of medicinal calcium chloride.

In order to achieve the purpose, the invention adopts the technical scheme that:

the first step is as follows: determination of the end-of-Evaporation temperature

Heating and evaporating a certain amount of refined calcium chloride solution to different temperature end points, drying the evaporated solution after tabletting, and detecting the purity and the pH value of the product so as to determine the evaporation termination temperature.

Furthermore, the evaporation termination temperature of the invention is controlled between 155 ℃ and 175 ℃.

The second step is that: determination of the amount of acid added by evaporation

Heating and evaporating a certain amount of refined calcium chloride solution, adding acid for three times in the evaporation process, controlling the acid adding amount in different stages, controlling the pH value of the evaporated solution to be 3-5, and then, testing the product purity and the pH value of the evaporated solution after flaking and drying.

Furthermore, the acid adding amount of the evaporated calcium chloride solution is controlled to be 0.2-0.8% (volume ratio) of the volume of the raw material solution.

The third step: determination of drying temperature

Heating and evaporating a certain amount of refined calcium chloride solution, cooling and flaking the evaporated solution, drying, and checking the purity and the pH value of the product according to different control drying temperatures.

Furthermore, the drying temperature of the invention is controlled between 180 ℃ and 200 ℃.

Fourth step of determining drying time

Heating and evaporating a certain amount of refined calcium chloride solution, cooling and tabletting an evaporated solution, drying, and checking the purity and the pH value of a product according to different drying times.

Furthermore, the drying time of the invention is controlled between 3 minutes and 10 minutes.

The invention has the technical effects that: the method can determine the acid-adding process parameters in the production process of the medicinal calcium chloride, determine the parameters in the optimal range, and produce the medicinal calcium chloride by the determined process parameters, thereby avoiding the influence of corrosion and the like on a production device caused by excessive acid-adding amount in the production process, and the influence of improper control of indexes such as evaporation temperature, time and the like on the production efficiency and the product quality, and further improving the production efficiency and the product purity.

Drawings

FIG. 1 is a schematic view of the process of the present invention.

Detailed Description

The invention is further described below with reference to the accompanying drawings. Referring to fig. 1, the process of the present invention is as follows:

1. determination of the end of vaporization

The purity of the product is determined by the height of the evaporation end point, and a certain amount of refined calcium chloride solution (W) is respectively taken in the invention_CaCl240-60 percent) is heated and evaporated to different temperature end points (155-175 ℃), and the evaporated liquid is subjected to flaking and drying to detect that the product contains pure. The results of the experiment are as follows:

according to the quality requirements of pharmacopoeia, the table shows that the evaporation end point is controlled at 155-175 ℃.

2. Determination of the amount of acid added by evaporation

Taking a certain amount of refined calcium chloride solution (W)_CaCl240-60%), adding acid in three steps in the evaporation process, controlling the pH value of the evaporation finished liquid to be 3-5, and detecting the pH value of the product after flaking and drying the evaporation finished liquid. The acid adding amount of the evaporated calcium chloride solution is controlled to be 0.2-0.8% (volume ratio) of the volume of the raw material solution. The test results are given in the following table:

as can be seen from the above, the acid addition amount of the calcium chloride solution should be controlled to be between 0.2 and 0.8 percent of the volume of the raw material liquid.

3. Determination of drying temperature

Taking a certain amount of refined calcium chloride solution (W)_CaCl240-60%), cooling the evaporated liquid, tabletting, drying, and detecting the purity and the pH value of the product according to different control drying temperatures (between 180 and 200 ℃). The results of the experiment are as follows:

as can be seen from the above table, the drying temperature is preferably controlled to be 180-200 ℃.

4. Determination of drying time

Taking a certain amount of refined calcium chloride solution (W)_CaCl240-60%), cooling the evaporated liquid, flaking, drying, and detecting the purity and the pH value of the product according to different drying times (between 3-10 minutes). The results of the experiment are as follows:

as can be seen from the above table, the drying time is preferably controlled to be 3-10 min.