WO2022247132A1

WO2022247132A1 - Continuous rectification apparatus and method used for silane coupling agent in photovoltaic industry

Info

Publication number: WO2022247132A1
Application number: PCT/CN2021/126601
Authority: WO
Inventors: 孙佳丽; 邱小魁; 李泽生; 陈�峰; 吴春近
Original assignee: 安徽硅宝有机硅新材料有限公司
Priority date: 2021-05-25
Filing date: 2021-10-27
Publication date: 2022-12-01
Also published as: DE112021000049T5; CN113230686A; CN113230686B

Abstract

A continuous rectification apparatus used for a silane coupling agent in the photovoltaic industry, comprising a peristaltic pump (1), a rectification still (3) and a packed tower (4). One end of the peristaltic pump (1) is connected to a heavy component storage tank (2), and the other end of the peristaltic pump (1) is divided into two paths to be connected to a lower middle portion of the packed tower (4) by means of a tee joint. The top of the packed tower (4) is connected to one end of a condenser (6), and the bottom of the packed tower (4) is connected to the rectification still (3). The rectification still (3) is connected to a vacuum pump (8). The other end of the condenser (6) is connected to a finished product receiving tank (7), and the finished product receiving tank (7) is connected to a buffer tank (9). A packing rotating assembly (5) is mounted in the packed tower (4). A backflushing assembly (10) is connected to the packing rotating assembly (5). The packing rotating assembly (5) rotates to adjust a channel in the packed tower (4), and the backflushing assembly (10) is used for backflushing cleaning of the packing rotating assembly (5).

Description

A kind of continuous rectification equipment and method applied to silane coupling agent in photovoltaic industry

technical field

The invention relates to the technical field of rectification equipment, in particular to a continuous rectification equipment and method applied to silane coupling agents in the photovoltaic industry.

Background technique

The silane coupling agent used in the photovoltaic industry has good weather resistance, sealing, electrical insulation, simple application process, and high efficiency. It has extremely high requirements for product purity and trace ion residues. On the one hand, ions will increase the electrical conductivity of the material. On the other hand, it will reduce the aging resistance and service life of the membrane material, so trace ion residues are required, the product purity is greater than 99.5%, free chlorine is less than 3ppm, and the acid value is less than 0.3mgKOH/g.

In the production process of silane coupling agent, it is necessary to remove the residual raw materials, solvents, salts, etc. in the heavy component before extracting the finished product. According to the different boiling points of each fraction, vacuum distillation equipment is generally used for purification, but manual operation is required for intermittent distillation. When the distillation of each batch of materials is completed, the operation of the equipment needs to be stopped before feeding and other operations, which will expose the product to air, and then partial hydrolysis will occur. It may lead to reduced product purity, greatly reduced rectification efficiency, and increased costs.

Contents of the invention

The object of the present invention is to provide a continuous rectification device and method for silane coupling agents used in the photovoltaic industry, so as to solve the problems raised in the above-mentioned background technology.

In order to achieve the above object, the present invention provides the following technical solution: a continuous rectification equipment applied to silane coupling agents in the photovoltaic industry, including a peristaltic pump, a rectification tank and a packed tower, one end of the peristaltic pump is connected to the heavy component storage tank , the other end of the peristaltic pump is connected to the middle and lower part of the packed tower in two ways through a tee, the top of the packed tower is connected to one end of the condenser, the bottom of the packed tower is connected to the rectification kettle, and the rectification kettle is connected to the vacuum pump, condensing The other end of the device is connected to the finished product receiving tank, and the finished product receiving tank is connected to the buffer tank;

The inner packing tower of the packing tower is equipped with a packing rotation assembly connected with a recoil assembly, the rotation of the packing rotation assembly is used to adjust the passage inside the packing tower, and the recoil assembly is used for recoil cleaning of the packing rotation assembly.

Further, the packing rotating assembly includes a rotating shaft, a partition, a support ring, a packing shell, an upper packing layer and a lower packing layer, and the supporting rings are fixed on the inner wall of the packing tower at equal intervals, and a A partition used to separate the left and right cavities of the packed tower. A movable rotating shaft runs through the center of the partition. The top of the rotating shaft passes through the packed tower to connect with the recoil assembly, and the rotating shaft between the partition and the partition A packing shell is installed on the top, and the upper and lower sides of the packing shell are respectively sealed and connected with the support rings at the upper and lower positions. The upper packing layer and the lower packing layer are fixed in the packing shell, and a cleaning chamber is formed between the upper packing layer and the lower packing layer.

Further, the rotating shaft is a hollow cylindrical member, and the branch pipe connected to the rotating shaft penetrates into the cleaning cavity of the stuffing shell and connects with the telescopic assembly.

Further, the recoil assembly includes a recoil pipe, a sleeve, a pillar and a power spindle. The port of the rotating shaft located outside the packed tower is inserted into the sleeve to seal and rotate. One end of the power spindle is fixed to the rotating shaft through the pillar, and the power spindle passes through the sleeve. It is fixed with the motor, and the recoil pipe is connected to the side of the sleeve. The liquid sprayed into the recoil pipe enters the interior of the rotating shaft, and the motor drives the power spindle and the rotating shaft to rotate synchronously.

Further, the telescopic assembly includes a spout, a spring and a sealing rod, one end of the sealing rod is fixed on the inner wall of the rotating shaft, the other end of the sealing rod extends into the branch pipe, the spring is sleeved on the sealing rod, one end of the spring is fixed to the spout, and the other end of the spring One end is fixed to the inner wall of the rotating shaft, and the sealing rod is inserted into the spout in the initial state to block the spring. The pressure generated by the water flowing in the recoil pipe flowing into the branch pipe makes the spout separate from the sealing rod, and the recoil liquid flows into the stuffing shell.

Another kind of technology that the present invention proposes, comprises the method for the continuous rectification equipment that is applied to the silane coupling agent of photovoltaic industry, comprises the following steps:

S1: The motor drives the rotating shaft to rotate to drive the packing shell to rotate, so that the upper packing layer and the lower packing layer block the passage from the peristaltic pump to the packing tower, and the multi-layer seal between the rectification kettle and the condenser;

S2: The peristaltic pump works to pump the material in the heavy component storage tank through the upper packing layer and the lower packing layer to filter and flow into the rectification kettle;

S3: The motor drives the rotation of the rotating shaft to drive the packing shell to rotate so that the upper packing layer and the lower packing layer block the channel between the rectification kettle and the condenser, and the multi-layer seal between the peristaltic pump and the packing tower;

S4: After the rectification kettle is heated, the steam generated by the rectification kettle is purified through the upper packing layer and the lower packing layer to condense in the condenser, and the liquid flows into the finished product receiving tank for storage;

S5: After the distillation is completed, the liquid flowing in the recoil pipe pushes the spout away from the sealing rod, and the recoil liquid flows into the packing shell to recoil clean the upper packing layer and the lower packing layer respectively.

Compared with prior art, the beneficial effect of the present invention is:

A continuous rectification equipment and method for silane coupling agents in the photovoltaic industry proposed by the present invention. The crude product with a certain liquid level is kept in the rectification kettle, and the inside of the distillation kettle is vacuumed with a vacuum pump, and the liquid is stirred. Heating, when the temperature at the top of the packed tower reaches 20-30°C, the material in the heavy component storage tank is injected into the system at a certain flow rate through the peristaltic pump, and rises with the steam to achieve the purification effect, and finally the gas phase silane coupling agent is cooled by the condenser After entering the finished product receiving tank, when the liquid level in the distillation tank exceeds the limit, it will be automatically discharged through the pump, and the two channels are controlled by the rotation of the power spindle and the rotating shaft. When one is opened, the other is closed, so that it can filter and recoil. In addition, the single-sided partition method is used to reduce the filling amount of the filler, and the spout is blocked by a spring, and it is in a closed state without external interference, so the steam cannot flow into the recoil pipe, and only the water flow pressure is greater than that of the spring. When it is elastic, push the nozzle to move, spray water into the cleaning chamber, complete the purpose of recoil cleaning, and design the optimal continuous distillation, which can greatly improve the distillation efficiency and product purity.

Description of drawings

Fig. 1 is the overall system diagram of the present invention;

Fig. 2 is a structural diagram of the packing rotating assembly of the present invention;

Fig. 3 is a rotating state diagram of the packing rotating assembly of the present invention;

Fig. 4 is the internal structural diagram of the packing rotating assembly of the present invention;

Fig. 5 is a structural diagram of the recoil assembly of the present invention;

Fig. 6 is a structural diagram of the telescopic assembly of the present invention.

In the figure: 1. Peristaltic pump; 2. Heavy component storage tank; 3. Rectification kettle; 4. Packed tower; 5. Packing rotating assembly; 51. Rotating shaft; 511. Branch pipe; ;54, packing shell; 55, upper packing layer; 56, lower packing layer; 57, telescopic assembly; 571, spout; 572, spring; 573, sealing rod; 6, condenser; 7, finished product receiving tank; 8, vacuum pump ; 9, buffer tank; 10, recoil assembly; 101, recoil pipe; 102, sleeve; 103, pillar;

Detailed ways

The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

Please refer to Figure 1, a continuous rectification equipment for silane coupling agents in the photovoltaic industry, including a peristaltic pump 1, a rectification tank 3 and a packed tower 4, one end of the peristaltic pump 1 is connected to the heavy component storage tank 2, and the peristaltic The other end of the pump 1 is connected to the middle and lower part of the packed tower 4 in two ways through a tee, and the feeding rate is controlled to 300-500L/h, which can realize continuous feeding, which greatly improves the processing efficiency and saves costs. The packed tower 4 The top of the condenser 6 is connected to one end of the condenser 6, the bottom of the packed tower 4 is connected to the rectifying still 3, the rectifying still 3 is connected to the vacuum pump 8, the other end of the condenser 6 is connected to the finished product receiving tank 7, and the finished product receiving tank 7 Connect with buffer tank 9.

Keep the crude product with a certain liquid level in the rectification tank 3, vacuumize the inside of the distillation tank with a vacuum pump 8, and stir and heat the liquid. When the temperature at the top of the packed tower 4 reaches 20-30°C, the recombined The components in the sub-storage tank 2 are injected into the system and rise with the steam to achieve the purification effect. Finally, the gas-phase silane coupling agent enters the finished product receiving tank 7 after being cooled by the condenser 6. When the liquid level in the rectifying tank 3 exceeds the limit It will be automatically discharged by a pump, and a temperature sensor and an air pressure sensor are installed in the rectifying kettle 3, the packed tower 4, the finished product receiving tank 7 and the buffer tank 9 to detect the internal temperature and air pressure.

Inside the packed tower 4, the packed tower 4 is equipped with a packing rotating assembly 5, and the packing rotating assembly 5 is connected with a recoil assembly 10. The packing rotating assembly 5 is rotated to adjust the inner channel of the packing tower 4, and the recoil assembly 10 is used for packing rotation. The recoil cleaning of component 5 uses its recoil cleaning method to perform internal quick cleaning to prolong its service life.

Please refer to Fig. 2-4, packing rotating assembly 5 comprises rotating shaft 51, dividing plate 52, supporting ring 53, packing case 54, upper packing layer 55 and lower packing layer 56, and supporting ring 53 is fixed on the packing column 4 at equal intervals On the inner wall, a partition 52 for separating the left and right cavities of the packed tower 4 is installed between the two support rings 53. A movable rotating shaft 51 runs through the center of the partition 52, and the top of the rotating shaft 51 passes through the packed tower. 4. It is connected with the recoil assembly 10, and the packing case 54 is installed on the rotating shaft 51 between the partition 52 and the partition 52. The rotating shaft 51 drives the packing case 54 to rotate. The ring 53 is sealed and connected, and the upper packing layer 55 and the lower packing layer 56 are fixed in the packing shell 54. A cleaning chamber is formed between the upper packing layer 55 and the lower packing layer 56. The thickness of the cleaning chamber is not more than 3 cm, so that the cleaning liquid can be divided into upper and lower parts. It flows into the upper packing layer 55 and the lower packing layer 56, thereby accomplishing the purpose of recoil cleaning.

The rotating shaft 51 is a hollow cylindrical member, and the branch pipe 511 connected to the rotating shaft 51 penetrates into the cleaning chamber of the packing case 54 and connects with the telescoping assembly 57 .

Please refer to Fig. 5, the recoil assembly 10 includes a recoil pipe 101, a sleeve 102, a pillar 103 and a power spindle 104, the rotating shaft 51 is located at the port outside the packed tower 4 and inserted into the sleeve 102 to seal and rotate, and one end of the power spindle 104 passes through the pillar 103 is fixed with the rotating shaft 51, the power main shaft 104 passes through the sleeve 102 and is fixed with the motor, the recoil pipe 101 is connected to the side of the sleeve 102, the liquid sprayed into the recoil pipe 101 enters the inside of the rotating shaft 51, and the motor drives the power The main shaft 104 and the rotating shaft 51 rotate synchronously, and the two channels are controlled by the rotation of the power main shaft 104 and the rotating shaft 51. When one is opened, the other is closed, so as to achieve the purpose of filtering and recoil, and adopts a single-sided partition method , reducing the filling amount of packing, and designing the optimal continuous distillation, which can greatly improve the distillation efficiency and product purity.

Please refer to Fig. 6, the telescopic assembly 57 includes a spout 571, a spring 572 and a sealing rod 573, one end of the sealing rod 573 is fixed on the inner wall of the rotating shaft 51, the other end of the sealing rod 573 extends into the branch pipe 511, and the spring 572 is sleeved on the sealing rod 511. On the rod 573, one end of the spring 572 is fixed to the spout 571, and the other end of the spring 572 is fixed to the inner wall of the rotating shaft 51. The spring 572 is inserted into the spout 571 to block the sealing rod 573 in the initial state, and the water flowing in the recoil pipe 101 flows into the branch pipe 511 The pressure generated inside makes the spout 571 separate from the sealing rod 573, and the recoil liquid flows into the stuffing shell 54, and the spout 571 is blocked by the spring 572, and it is in a closed state without external interference, so the steam cannot flow into the recoil pipe 101 , only when the pressure of the water flow is greater than the elastic force of the spring 572, the nozzle 571 is pushed to move, and the water flow is sprayed into the cleaning chamber to complete the purpose of recoil cleaning.

The method applied to the continuous rectification equipment of silane coupling agent in photovoltaic industry comprises the following steps:

Step 1: The motor drives the rotating shaft 51 to rotate to drive the packing shell 54 to rotate so that the upper packing layer 55 and the lower packing layer 56 block the passage from the peristaltic pump 1 to the packing tower 4, and the multi-layer seal between the rectifying kettle 3 and the condenser 6;

Step 2: The peristaltic pump 1 works to extract the material in the heavy component storage tank 2 to pass through the upper packing layer 55 and the lower packing layer 56 to filter and flow into the rectifying kettle 3;

Step 3: The motor drives the rotating shaft 51 to rotate to drive the packing shell 54 to rotate so that the upper packing layer 55 and the lower packing layer 56 block the channel between the rectification kettle 3 and the condenser 6, and the multi-layer seal between the peristaltic pump 1 and the packing tower 4;

Step 4: After the rectification kettle 3 is heated, the steam generated by the rectification kettle 3 is purified through the upper packing layer 55 and the lower packing layer 56 to be condensed in the condenser 6, and the liquid flows into the finished product receiving tank 7 for storage;

Step 5: After the distillation is completed, the liquid flowing in the recoil pipe 101 pushes the nozzle 571 away from the sealing rod 573, and the recoil liquid flows into the packing shell 54 to recoil clean the upper packing layer 55 and the lower packing layer 56 respectively.

The tower height of the packed tower 4 is 6000mm, and the diameter is 500mm. There are 3 tower sections in total, and the height of each tower is 2000mm. Connect the heavy component storage tank 2, the purity of the heavy component of the silane coupling agent is greater than 98%, and the product detection data obtained by rectification is as follows:

The advantage is that the concept is novel, the design is reasonable, and the operation is safe. The rectification tank 3 is designed for continuous feeding, and the height of the packed tower 4 is appropriately increased, which is beneficial to the separation of the silane coupling agent in the rectification tank 3, and improves product purity and company income. .

In summary; the present invention is applied to the continuous rectification equipment and method of silane coupling agent in the photovoltaic industry, the crude product of certain liquid level is kept in rectification still 3, vacuumizes the inside of still still with vacuum pump 8, and Stir and heat the liquid. When the temperature at the top of the packed tower 4 reaches 20-30°C, the material in the heavy component storage tank 2 is pumped into the system through the peristaltic pump 1, and rises with the steam to achieve the purification effect. Finally, the gas phase silane coupling agent After being cooled by the condenser 6, it enters the finished product receiving tank 7. When the liquid level in the rectification kettle 3 exceeds the limit, it will be automatically discharged through the pump. The two channels are controlled by the rotation of the power spindle 104 and the rotating shaft 51. When one is opened, the other is closed. , so as to achieve the purpose of filtering and recoil, and adopt the single-sided partition method to reduce the filling amount of the filler, and use the spring 572 to block the spout 571, and it is in a closed state without external interference, so the steam cannot When it flows into the recoil pipe 101, only when the pressure of the water flow is greater than the elastic force of the spring 572, the spout 571 is pushed to move, and the water flow is sprayed into the cleaning chamber to complete the purpose of recoil cleaning. The optimal continuous rectification is designed, which can greatly improve the Improve distillation efficiency and improve product purity.

The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Anyone familiar with the technical field within the technical scope disclosed in the present invention, according to the technical solution of the present invention Any equivalent replacement or change of the inventive concepts thereof shall fall within the protection scope of the present invention.

Claims

A continuous rectification device applied to silane coupling agents in the photovoltaic industry, characterized in that it includes a peristaltic pump (1), a rectification kettle (3) and a packed tower (4), and one end of the peristaltic pump (1) is connected to the heavy component The storage tank (2) is connected, the other end of the peristaltic pump (1) is connected to the middle and lower part of the packed tower (4) in two ways through a tee, and the top of the packed tower (4) is connected to one end of the condenser (6). The bottom of the packed tower (4) is connected to the rectifying kettle (3), the rectifying kettle (3) is connected to the vacuum pump (8), the other end of the condenser (6) is connected to the finished product receiving tank (7), and the finished product receives Tank (7) is connected with surge tank (9);

The inner packing tower (4) of the packing tower (4) is equipped with a packing rotating assembly (5), and a recoil assembly (10) is connected to the packing rotating assembly (5), and the packing rotating assembly (5) is rotated to adjust the packing The channel inside the tower (4) and the recoil assembly (10) are used for recoil cleaning of the packing rotating assembly (5).
A continuous rectification device applied to silane coupling agents in the photovoltaic industry according to claim 1, characterized in that the packing rotating assembly (5) includes a rotating shaft (51), a partition (52), a support ring (53 ), the packing shell (54), the upper packing layer (55) and the lower packing layer (56), the support rings (53) are fixed on the inner wall of the packed tower (4) at equal intervals, and the two support rings (53) A partition (52) for separating the left and right cavities of the packed tower (4) is installed between them. A movable rotating shaft (51) runs through the center of the partition (52), and the top of the rotating shaft (51) passes through The packed tower (4) is connected to the recoil assembly (10), and a packing shell (54) is installed on the rotating shaft (51) between the partition (52) and the partition (52), and the upper and lower sides of the packing shell (54) The two sides are respectively sealed and connected with the support rings (53) at the upper and lower positions, the upper packing layer (55) and the lower packing layer (56) are fixed in the packing shell (54), and the upper packing layer (55) and the lower packing layer (56) A cleaning chamber is formed between them.
A kind of continuous rectification equipment applied to silane coupling agent in photovoltaic industry as claimed in claim 2, characterized in that, the rotating shaft (51) is a hollow cylindrical member, and the branch pipe connected to the rotating shaft (51) (511) penetrates into the cleaning cavity of the stuffing case (54) and joins with the telescopic assembly (57).
A continuous rectification device applied to silane coupling agents in the photovoltaic industry according to claim 3, characterized in that the recoil assembly (10) includes a recoil pipe (101), a sleeve (102), a pillar (103 ) and the power spindle (104), the rotating shaft (51) is located outside the packed tower (4) and inserted into the sleeve (102) to seal and rotate, and one end of the power spindle (104) is fixed to the rotating shaft (51) through the pillar (103) , the power spindle (104) passes through the sleeve (102) and is fixed to the motor, the recoil pipe (101) is connected to the side of the sleeve (102), and the liquid sprayed into the recoil pipe (101) enters the rotating shaft (51 ) inside, the motor drives the power main shaft (104) and the rotating shaft (51) to rotate synchronously.
A kind of continuous rectification equipment applied to silane coupling agent in photovoltaic industry as claimed in claim 4, characterized in that the telescopic assembly (57) includes a spout (571), a spring (572) and a sealing rod (573), and the sealing One end of the rod (573) is fixed on the inner wall of the rotating shaft (51), the other end of the sealing rod (573) extends into the branch pipe (511), the spring (572) is sleeved on the sealing rod (573), and the spring (572) One end is fixed to the spout (571), the other end of the spring (572) is fixed to the inner wall of the rotating shaft (51), the spring (572) is inserted into the spout (571) in the initial state to block the sealing rod (573), and the recoil pipe (101 ) flows into the branch pipe (511) to generate pressure that causes the spout (571) to break away from the sealing rod (573), and the recoil fluid flows into the stuffing shell (54).
A continuous rectification method applied to the continuous rectification equipment of photovoltaic industry silane coupling agent as claimed in claim 5, is characterized in that, comprises the following steps:

S1: The motor drives the rotating shaft (51) to rotate to drive the packing shell (54) to rotate so that the upper packing layer (55) and the lower packing layer (56) block the passage from the peristaltic pump (1) to the packing tower (4), and the rectification kettle ( 3) Multi-layer sealing between the condenser (6);

S2: The peristaltic pump (1) works to pump the material in the heavy component storage tank (2) through the upper packing layer (55) and the lower packing layer (56) to filter and flow into the rectifying kettle (3);

S3: The motor drives the rotating shaft (51) to rotate to drive the packing shell (54) to rotate so that the upper packing layer (55) and the lower packing layer (56) block the channel between the rectification kettle (3) and the condenser (6), and the peristaltic pump (1) Multi-layer sealing between the packed tower (4);

S4: After the rectification kettle (3) is heated, the steam generated by the rectification kettle (3) is purified through the upper packing layer (55) and the lower packing layer (56) to be condensed in the condenser (6), and the liquid flows into the finished product receiving tank (7 ) internal storage;

S5: After the distillation is completed, the liquid flowing in the recoil pipe (101) pushes the spout (571) away from the sealing rod (573), and the recoil liquid flows into the packing shell (54) to face the upper packing layer (55) and the lower packing layer respectively (56) Recoil cleaning.