CN216396331U - Device for preparing alpha semi-hydrated phosphogypsum - Google Patents

Abstract

The utility model provides a device for preparing alpha hemihydrate phosphogypsum, which comprises a heating device, wherein the heating device is provided with a reaction device, three ports are formed above the reaction device, and a condensing device, a stirring device and a temperature sensor are respectively connected and arranged on the reaction device; the condensing device is provided with a water inlet pipe and a water outlet pipe; the stirring device is provided with a tetrafluoroethylene stirring paddle; the temperature sensor is connected with the heating device. The heating device adopts a digital display constant temperature electric heating jacket; the reaction device adopts a three-mouth flask; the condensing device adopts a spherical condensing pipe; the stirring device adopts a precise electric stirrer; when the method is used, firstly, a salt medium solution is added from a bottle opening, a thermocouple is inserted, a stirrer and an electric heating sleeve switch are turned on for heating, after the set temperature is reached, the raw material phosphogypsum is added to start reaction, so that the phosphogypsum is converted into an alpha hemihydrate phosphogypsum product, the preparation of the alpha hemihydrate phosphogypsum under the normal pressure condition is realized, the reaction condition in the bottle can be directly observed easily, the real-time sampling is realized, and the reaction temperature and the stirring speed can be accurately controlled.

Description

Device for preparing alpha semi-hydrated phosphogypsum

Technical Field

The utility model relates to an experimental device for preparing alpha hemihydrate phosphogypsum, and belongs to the field of comprehensive utilization of resources.

Background

Phosphogypsum is a large amount of industrial solid waste discharged in the wet-process phosphoric acid production process, and the yield of phosphogypsum in China reaches 7500 million tons in 2019. The main component of the phosphogypsum is dihydrate gypsum, and the phosphogypsum also contains impurities such as phosphorus, fluorine, organic matters and the like, so that the phosphogypsum has high utilization difficulty and low comprehensive utilization rate. In 2006, the national general environmental protection agency qualitatively determines the phosphogypsum as dangerous solid waste, and in 2018, Guizhou province proposes comprehensively implementing the phosphogypsum to use for fixed production, so as to realize the production and consumption balance of the phosphogypsum. The stockpiling of the phosphogypsum not only occupies a large amount of land resources, but also causes serious environmental pollution. Therefore, how to accelerate the resource utilization of the phosphogypsum is the focus of the current research.

In Chinese patent literature, the utility model patent with the publication number of CN104628274A discloses a method for preparing high-strength alpha hemihydrate gypsum by phosphogypsum, which comprises the steps of mixing phosphogypsum, pretreatment additive, water and crystal modifier, uniformly stirring, ageing, pelletizing, and then completing steam curing and drying in a still kettle to prepare the high-strength alpha hemihydrate gypsum.

The alpha hemihydrate gypsum is a cementing material with excellent performance, and the preparation of the alpha hemihydrate gypsum by taking the phosphogypsum as a raw material is an important way for high added value utilization of the alpha hemihydrate gypsum. In industrial production, the alpha hemihydrate gypsum is prepared by adopting an evaporation method and a pressurized aqueous solution method, but the method needs high-temperature and high-pressure equipment, the reaction process is difficult to control, and the product quality is unstable. Because the reaction condition is mild, the normal-pressure hydrothermal method for preparing the alpha hemihydrate phosphogypsum has good application prospect. Therefore, it is necessary to develop an experimental device for preparing alpha hemihydrate phosphogypsum under normal pressure conditions.

SUMMERY OF THE UTILITY MODEL

The utility model aims to overcome the defects of the prior art and provides an experimental device for preparing alpha hemihydrate phosphogypsum, which is convenient to operate, easy to directly observe the reaction condition in a bottle and sample in real time, and also capable of accurately controlling the reaction temperature and the stirring speed.

The technical scheme of the utility model is that the device for preparing alpha semi-hydrated phosphogypsum comprises a heating device, wherein a reaction device is arranged on the heating device, three ports are formed above the reaction device, and a condensing device, a stirring device and a temperature sensor are respectively connected and arranged on the reaction device; the condensing device is provided with a water inlet pipe and a water outlet pipe; the stirring device is provided with a tetrafluoroethylene stirring paddle; the temperature sensor is connected with the heating device.

The heating device adopts a digital display constant temperature electric heating jacket, the temperature sensor adopts a thermocouple, and the thermocouple is inserted into reaction slurry in the reaction device. The reaction device adopts a three-neck flask, and the bottleneck of the three-neck flask is provided with a polytetrafluoroethylene plug for sealing; the salt solution and the phosphogypsum are added from the bottle mouth of the three-neck flask, and slurry is also sucked from the bottle mouth in the reaction process. The condensing device adopts a spherical condensing pipe, the lower end of the condensing pipe is a water inlet connected with a water inlet pipe, the upper end of the condensing pipe is a water outlet connected with a water outlet pipe, and the water inlet pipe and the water outlet pipe adopt latex pipes. The stirring device adopts a precise electric stirrer.

Compared with the prior art, the utility model has the following beneficial effects:

the device for preparing the alpha hemihydrate phosphogypsum can quickly prepare the alpha hemihydrate phosphogypsum under the normal pressure condition, can directly observe the condition of the whole reaction process, can extract a reaction sample for analyzing the dehydration kinetics of the phosphogypsum, and immediately judges whether the reaction is finished.

Drawings

FIG. 1 is a schematic diagram of the apparatus of the present invention.

The labels in the figures are: 1-heating device, 2-reaction device, 3-condensing device, 4-stirring device, 5-temperature sensor, 6-polytetrafluoroethylene plug, 7-bottle mouth, 8-tetrafluoroethylene stirring paddle, 9-water outlet pipe and 10-water inlet pipe.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the description of the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.

As shown in FIG. 1, the apparatus of the present invention is mainly composed of a heating apparatus 1, a reaction apparatus 2, a condensing apparatus 3, a stirring apparatus 4 and a temperature sensor 5. The heating device 1 is a digital display constant-temperature electric heating jacket and is provided with a temperature sensor 5 for detecting the temperature of reaction slurry in real time, the temperature sensor 5 adopts a thermocouple and needs to be inserted into the reaction slurry, and the temperature control precision is +/-1 ℃; the reaction temperature may be set to normal temperature to 100 ℃ according to the experimental requirements.

The reaction device 2 adopts a three-mouth flask, and the mouth of the flask is sealed by a polytetrafluoroethylene plug 6; according to the volume of the required reaction slurry, three-neck flasks with different volumes such as 250mL, 500mL, 1000mL, 2000mL, 5000mL and the like can be selected and matched with digital display constant temperature electric heating jackets with corresponding specifications for use, and the three-neck flasks are flatly placed in the digital display constant temperature electric heating jackets in the use process. The condensing device 3 adopts a spherical condensing tube, the effective length is more than 30cm, the caliber is 24mm, and the condensing tube is inserted into any bottle mouth at two sides of the three-neck flask; tap water inlet and outlet are arranged at the upper end and the lower end of the condenser pipe, a water inlet is arranged at the lower end, a water outlet is arranged at the upper end, and the condenser pipe and the water inlet are respectively connected by latex pipes, wherein the latex pipes have the specifications of 6mm inner diameter and 9mm outer diameter. The stirring device 4 adopts a precise electric stirrer, is matched with a polytetrafluoroethylene stirring paddle 8, and the stirring paddle is deeply inserted into the middle lower part of the reaction slurry in the using process, so that the slurry cannot be precipitated.

During the test operation, the salt solution and phosphogypsum are added from the mouth 7 of the three-neck flask, and the slurry is also sucked from the mouth 7 during the reaction.

As shown in fig. 1, the specific steps for preparing alpha-hemihydrate phosphogypsum by adopting the utility model are as follows:

1) horizontally placing a 500mL three-neck flask into a digital display constant temperature electric heating jacket, vertically inserting a polytetrafluoroethylene stirring paddle 8 into the bottom of the three-neck flask from a middle bottle opening 7, wherein the polytetrafluoroethylene stirring paddle cannot contact the bottom of the flask, the upper end of the polytetrafluoroethylene stirring paddle is fixed on a motor of a precise electric stirrer, and a gap between a stirring rod and the bottle opening is sealed by a polytetrafluoroethylene plug 6;

2) inserting a spherical condenser pipe with the effective length of 50cm into the rightmost bottle mouth of the three-neck flask for fixation, wherein the upper end and the lower end of the condenser pipe are respectively connected with a latex pipe, the lower end is a tap water inlet, the upper end is a water outlet, a tap is opened, tap water forms counter flow in the condenser pipe, and water can not be cut off in the whole reaction process;

3) adding 400mL of 15 mass percent sodium chloride solution into a three-neck flask through a bottle opening 7, inserting a thermocouple sleeved with a polytetrafluoroethylene plug 6 into the solution, turning on a precise electric stirrer and an electric heating sleeve switch, and setting the stirring speed to be 200 r/min;

4) when the temperature of the solution reaches 95 ℃, 100g of phosphogypsum is added into a three-neck flask through a bottle opening 7, the reaction is carried out for 120min at constant temperature, the reaction condition in the bottle can be directly observed in the reaction process, about 20mL of reaction slurry can be sucked from the bottle opening 7 by a rubber head dropper, and the reaction condition and the content of crystal water for measuring the product are observed by a microscope;

5) after the reaction is finished, the electric heating sleeve and the precise electric stirrer are closed, the electric thermocouple, the condensing pipe and the stirring paddle are removed, the slurry is quickly filtered, washed by boiling water and dried to obtain the long columnar alpha semi-hydrated phosphogypsum product, and the filtrate can be recycled after being treated.

The above embodiments are merely illustrative of the technical idea of the present invention, and it is apparent to those skilled in the art that the present invention is not limited to the details of the above embodiments and can be embodied in other specific forms without departing from the spirit or essential characteristics of the utility model. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the utility model being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (5)

1. A device for preparing alpha hemihydrate phosphogypsum is characterized in that: the device comprises a heating device (1), wherein a reaction device (2) is arranged on the heating device (1), three openings are formed above the reaction device (2), and a condensing device (3), a stirring device (4) and a temperature sensor (5) are respectively connected and arranged; the condensing device (3) is provided with a water inlet pipe (10) and a water outlet pipe (9); the stirring device (4) is provided with a tetrafluoroethylene stirring paddle (8); the temperature sensor (5) is connected with the heating device (1).

2. The plant for the preparation of alpha hemihydrate phosphogypsum according to claim 1, characterized in that: the heating device (1) adopts a digital display constant temperature electric heating jacket, the temperature sensor (5) adopts a thermocouple, and the thermocouple is inserted into the reaction slurry in the reaction device (2).

3. The plant for the preparation of alpha hemihydrate phosphogypsum according to claim 1, characterized in that: the reaction device (2) adopts a three-mouth flask, and a bottle mouth (7) of the three-mouth flask is provided with a polytetrafluoroethylene plug (6) for sealing; the salt solution and the phosphogypsum are added from the bottle mouth (7) of the three-neck flask, and slurry is also sucked from the bottle mouth (7) in the reaction process.

4. The plant for the preparation of alpha hemihydrate phosphogypsum according to claim 1, characterized in that: condensing equipment (3) adopts spherical condenser pipe, and the lower extreme is water inlet connection inlet tube (10), and the upper end is delivery port connection outlet pipe (9), emulsion tube is adopted in inlet tube (10) and outlet pipe (9).

5. The plant for the preparation of alpha hemihydrate phosphogypsum according to claim 1, characterized in that: the stirring device (4) adopts a precise electric stirrer.

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