阅读说明：本技术 一种核纯级硼酸标准物质制备装置 (Nuclear pure grade boric acid standard substance preparation device ) 是由 郭国龙 王春叶 王海珍 杨丹丹 孙雪云 龚明明 李梁 于 2019-10-16 设计创作，主要内容包括：本发明涉及硼酸标准物质制备技术领域,具体公开了一种核纯级硼酸标准物质制备装置,通过加热系统内部的加压泵可将油浴锅里的导热油泵入到釜体的玻璃夹层中,使夹层中充满导热油,通过热的导热油对整个釜体进行加热。本发明装置结构简单,能够用于硼酸标准物质的制备,制备的标准物质技术指标满足相关要求。(The invention relates to the technical field of boric acid standard substance preparation, and particularly discloses a device for preparing a nuclear pure grade boric acid standard substance. The device has a simple structure, can be used for preparing the boric acid standard substance, and the technical indexes of the prepared standard substance meet the relevant requirements.)

1. The utility model provides a pure grade boric acid standard substance preparation facilities of nuclear which characterized in that: comprises a feed valve (1), a snakelike condenser pipe (2), a liquid collecting bottle (3), a circulating water vacuum pump (4), a vacuum pressure gauge (5), a heating system (6), a kettle body (7), a temperature sensor (8), a variable frequency motor (9), a polytetrafluoroethylene stirrer (10) and a discharge valve (11);

the kettle body (7) is a double-layer glass reaction kettle;

the feeding valve (1) is arranged at a feeding port at the upper part of the kettle body (7), and raw materials required for producing boric acid standard substances are added into the kettle body (7) by unscrewing the feeding valve (1);

the liquid collecting bottle (3) is communicated with the upper part of the inside of the kettle body (7) through a pipeline, and a snake-shaped condensing pipe (2) is arranged above the liquid collecting bottle (3) and can condense and collect evaporated moisture;

the variable frequency motor (9) is arranged above the kettle body (7), and the lower end of the variable frequency motor (9) is connected with a polytetrafluoroethylene stirrer (10) for stirring boric acid in the kettle body (7) to achieve the purpose of sample uniformity;

the circulating water vacuum pump (4) is used for controlling the pressure inside the kettle body (7) and accelerating the evaporation of water in the preparation process in a vacuum negative pressure mode;

the vacuum pressure gauge (5) is used for monitoring the pressure inside the kettle body (7) in real time;

the heating system (6) is used for heating the whole kettle body (7);

the temperature in the kettle body (7) is measured by a temperature sensor (8);

a discharge valve (11) is arranged at a discharge port at the bottom of the kettle body (7), and the prepared boric acid standard substance is discharged by unscrewing the discharge valve (11).

2. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 1, wherein: the heating system (6) is a high-temperature circulating oil bath, heat conducting oil in the oil bath can be pumped into the glass interlayer of the kettle body (7) through a pressure pump in the oil bath, the interlayer is filled with the heat conducting oil, and the whole kettle body (7) is heated through the hot heat conducting oil.

3. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 2, wherein: the bottom of the liquid collecting bottle (3) is provided with a water outlet which is sealed by a ground glass plug and used for discharging collected water.

4. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 3, wherein: the feed valve (1) is a polyethylene knob with a soft gasket, so that a feed port can be prevented from being corroded by water and acid mist, and the soft gasket is used for improving the sealing property;

the discharge valve (11) is a polyethylene knob with a soft gasket, so that the discharge port can be prevented from being corroded by water and acid mist, and the soft gasket is used for increasing the sealing property.

5. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 4, wherein: the charging valve (1) is fixed at the charging port of the kettle body (7) by four screws, and has uniform stress and good sealing property;

the discharge valve (11) is fixed at the discharge port of the kettle body (7) by four screws, and has uniform stress and good sealing property.

6. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 5, wherein: the reaction speed is controlled by controlling the rotation speed of the polytetrafluoroethylene stirrer (10).

7. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 6, wherein: the stirring speed of the variable frequency motor (9) is 0-130 r/min.

8. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 7, wherein: the vacuum pressure value in the kettle body (7) is-0.085 to-0.095 Mpa.

9. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 8, wherein: the temperature in the kettle body (7) is kept at 50-55 ℃.

10. The apparatus for preparing a nuclear-pure grade boric acid standard substance according to claim 9, wherein: the stirring speed of the variable frequency motor (9) is 120r/min, the vacuum pressure value in the kettle body (7) is-0.090 Mpa, and the temperature in the kettle body (7) is kept at 52 ℃.

Technical Field

The invention belongs to the technical field of preparation of standard boric acid substances, and particularly relates to a device for preparing a standard boric acid substance with a pure nuclear grade.

Background

The water is a main carrier of the primary loop coolant of the pressurized water reactor, the pH value in the water has great influence on the corrosion rate of equipment and materials, and the pH value of the primary loop coolant can be controlled to be alkalescent by adjusting boric acid and lithium hydroxide, so that the corrosion rate of stainless steel materials is lowest. However, harmful impurities in the primary loop water threaten the safe operation of the reactor through various forms, such as the existence of iron, calcium, magnesium and other ions, and the nuclear power station has strict limits on impurity elements such as iron, calcium, magnesium, chlorine, fluorine, sulfate and the like in boric acid.

At present, no boric acid standard substance matching the content of impurity elements such as iron, calcium, magnesium, chlorine, fluorine, sulfate radical and the like exists in China.

Therefore, it is necessary to develop a device for preparing a nuclear pure grade boric acid standard substance.

Disclosure of Invention

The invention aims to provide a device for preparing a standard substance of nuclear pure grade boric acid, which can produce the standard substance of the nuclear pure grade boric acid meeting the requirements.

The technical scheme of the invention is as follows:

a device for preparing a nuclear pure grade boric acid standard substance comprises a feed valve, a snakelike condenser pipe, a liquid collecting bottle, a circulating water vacuum pump, a vacuum pressure gauge, a heating system, a kettle body, a temperature sensor, a variable frequency motor, a polytetrafluoroethylene stirrer and a discharge valve;

the kettle body is a double-layer glass reaction kettle;

the feeding valve is arranged at a feeding port at the upper part of the kettle body, and raw materials required for producing boric acid standard substances are added into the kettle body by unscrewing the feeding valve;

the liquid collecting bottle is communicated with the upper part of the interior of the kettle body through a pipeline, and a snake-shaped condensing pipe is arranged above the liquid collecting bottle and can condense and collect evaporated moisture;

the variable frequency motor is arranged above the kettle body, and the lower end of the variable frequency motor is connected with a polytetrafluoroethylene stirrer for stirring boric acid in the kettle body to achieve the purpose of sample uniformity;

the circulating water vacuum pump is used for controlling the pressure inside the kettle body and accelerating the evaporation of water in the preparation process in a vacuum negative pressure mode;

the vacuum pressure gauge is used for monitoring the pressure in the kettle body in real time;

the heating system is used for heating the whole kettle body;

the temperature in the kettle body is measured by a temperature sensor;

and a discharge valve is arranged at a discharge port at the bottom of the kettle body, and the prepared boric acid standard substance is discharged by unscrewing the discharge valve.

The heating system is a high-temperature circulating oil bath, heat conducting oil in the oil bath can be pumped into the glass interlayer of the kettle body through the pressure pump in the heating system, so that the interlayer is filled with the heat conducting oil, and the whole kettle body is heated through the hot heat conducting oil.

The bottom of the liquid collecting bottle is provided with a water outlet which is sealed by a ground glass plug and used for discharging the collected water.

The feed valve is a polyethylene knob with a soft gasket, so that the feed port can be prevented from being corroded by water and acid mist, and the soft gasket is used for improving the sealing property;

the baiting valve be the polyethylene material knob that has the soft gasket, can prevent that the drain hole from being corroded by water and acid mist, the soft gasket be used for increasing the leakproofness.

The charging valve is fixed at the charging port of the kettle body by four screws, and has uniform stress and good sealing property;

the material discharging valve is fixed at the material discharging opening of the kettle body by four screws, and has uniform stress and good sealing property.

The reaction speed is controlled by controlling the rotation speed of the polytetrafluoroethylene stirrer.

The stirring speed of the variable frequency motor is 0-130 r/min.

The vacuum pressure value in the kettle body is-0.085 to-0.095 Mpa.

The temperature in the kettle body is kept at 50-55 ℃.

The stirring speed of the variable frequency motor is 120r/min, the vacuum pressure value in the kettle body is-0.090 Mpa, and the temperature in the kettle body is kept at 52 ℃.

The invention has the following remarkable effects:

the invention provides a device for preparing a nuclear pure grade boric acid standard substance, which is simple in structure and can be used for preparing the boric acid standard substance, and the technical indexes of the prepared standard substance meet the relevant requirements.

Drawings

FIG. 1 is a schematic diagram of a device for preparing a nuclear pure grade boric acid standard substance.

In the figure: 1. a feed valve; 2. a serpentine condenser tube; 3. a liquid collection bottle; 4. a circulating water vacuum pump; 5. a vacuum pressure gauge; 6. a heating system; 7. a kettle body; 8. a temperature sensor; 9. a variable frequency motor; 10. a polytetrafluoroethylene stirrer; 11. a discharge valve.

Detailed Description

The invention is described in further detail below with reference to the figures and the embodiments.

The device for preparing the nuclear pure grade boric acid standard substance shown in figure 1 comprises a charging valve 1, a snakelike condenser pipe 2, a liquid collecting bottle 3, a circulating water vacuum pump 4, a vacuum pressure gauge 5, a heating system 6, a kettle body 7, a temperature sensor 8, a variable frequency motor 9, a polytetrafluoroethylene stirrer 10 and a discharge valve 11.

The kettle body 7 is a double-layer glass reaction kettle.

The feed valve 1 is arranged at the feed inlet at the upper part of the kettle body 7, and raw materials required for producing boric acid standard substances are added into the kettle body 7 by unscrewing the feed valve 1.

The charge valve 1 for the polyethylene material knob that has the soft gasket, can prevent that the charge door from being corroded by water and acid mist, the soft gasket be used for increasing the leakproofness.

The charging valve 1 can be fixed at the charging port of the kettle body 7 by four screws, and has uniform stress and good sealing property.

The liquid collecting bottle 3 is communicated with the upper part of the inner part of the kettle body 7 through a pipeline, and the snake-shaped condensing pipe 2 is arranged above the liquid collecting bottle 3 and can condense and collect evaporated moisture.

The liquid collecting bottle 3 is 5L in volume, a water outlet is formed in the bottom of the liquid collecting bottle, and the liquid collecting bottle is plugged by a ground glass plug and used for discharging collected water.

The variable frequency motor 9 is arranged above the kettle body 7, and the lower end of the variable frequency motor 9 is connected with a polytetrafluoroethylene stirrer 10 for stirring boric acid in the kettle body 7 to achieve the purpose of sample homogenization. Meanwhile, the reaction speed can be controlled by controlling the rotation speed of the polytetrafluoroethylene stirrer 10.

The stirring speed of the variable frequency motor 9 is 110-130 r/min, and preferably 120 r/min.

The circulating water vacuum pump 4 is used for controlling the pressure inside the kettle body 7 and accelerating the evaporation of water in the preparation process in a vacuum negative pressure mode.

The vacuum pressure gauge 5 is used for monitoring the pressure inside the kettle body 7 in real time, and ensuring that the vacuum pressure value inside the kettle body 7 is-0.085 to-0.095 Mpa, preferably-0.090 Mpa.

The heating system 6 is a high-temperature circulating oil bath, heat conducting oil in the oil bath can be pumped into the glass interlayer of the kettle body 7 through a pressure pump in the high-temperature circulating oil bath, the interlayer is filled with the heat conducting oil, the whole kettle body 7 is heated through the hot heat conducting oil, and the temperature in the kettle body 7 is kept at 50-55 ℃, preferably 52 ℃.

The temperature in the kettle body 7 is measured by a temperature sensor 8.

A discharge valve 11 is arranged at a discharge port at the bottom of the kettle body 7, and the prepared boric acid standard substance is discharged by unscrewing the discharge valve 11.

The baiting valve 11 is a polyethylene knob with a soft gasket, so that the baiting hole can be prevented from being corroded by water and acid mist, and the soft gasket is used for increasing the sealing property.

The discharge valve 11 can be fixed at the discharge port of the kettle body 7 by four screws, and has uniform stress and good sealing property.