A method and equipment for preparing block silicone oil softener

Abstract

The invention belongs to the field of chemical processing technology, and specifically relates to a method for preparing a block silicone oil softener and a device thereof. Through the production method of the softener of the present invention, the production efficiency can be improved, the block silicone oil softener can be produced with relatively simple production steps, the production steps and processes can be reduced, and the softener can be ensured to have good quality; through the setting of a reflux reaction mechanism, when the reflux reaction is carried out, the steam in the tank body can be effectively condensed to improve the reaction effect, and the stirring of the solvent can be synchronized with the pumping of the cooling liquid, and further, the steam in the tank body can be assisted to accelerate the flow to improve the efficiency and effect of condensation; the setting of the filtering mechanism can further cooperate with the stirring action to filter the impurities in the solvent to improve the purity of the solvent.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical processing, and in particular relates to a preparation method and equipment of a block silicone oil softener. Background Art

[0002] Softener refers to a production auxiliary that can make the surface of textile fibers smooth and make the product more comfortable. With the development of the chemical industry, silicone softeners are currently widely used in the textile industry due to their unique properties and effects.

[0003] At present, in the production process of block modified silicone oil softeners, in order to improve the purity of block silicone oil and ensure sufficient reaction of solvent, most of them require more complicated processing steps to meet the above requirements. However, this method, on the one hand, causes a long processing cycle and does not meet the needs of efficient production. On the other hand, when the solvent undergoes a critical reflux reaction, processing problems such as insufficient reaction and high energy consumption are prone to occur, resulting in high production energy consumption and difficult to control product quality. Summary of the invention

[0004] The purpose of the present invention is to provide a method for preparing a block silicone oil softener and an apparatus thereof, so as to solve the problems mentioned in the background technology.

[0005] In order to achieve the above technical objectives, the technical solution adopted by the present invention is as follows:

[0006] A method for preparing a block silicone oil softener, the specific preparation steps are as follows:

[0007] Step 1: Prepare the epoxy-terminated double-capped end, any one of DMC or D4 and the catalyst required for the reaction;

[0008] Step 2: Add any one of the end epoxy double head, DMC or D4 and a catalyst into the tank body for reaction, wherein the reaction environment is heat preservation reaction and vacuumization, wherein the heating is continuously increased during the vacuuming process until the vacuum is completely obtained and then the heat is maintained to obtain the end epoxy silicone oil;

[0009] Step 3: Add the end epoxy silicone oil and the catalyst in step 2 into the tank body for reaction, wherein the reaction environment is a heat preservation reaction and a reflux reaction is carried out simultaneously, and finally the solvent is replaced to obtain the block silicone oil.

[0010] The DMC is dimethyl carbonate, the D4 is octamethylcyclotetrasiloxane, and the catalyst comprises dimethylacetamide, a base catalyst, polyetheramine ED-900 and isopropyl alcohol.

[0011] The catalysts used in step 2 and added in sequence are dimethylacetamide and a base catalyst.

[0012] The catalysts used in step 3 and added in sequence are polyetheramine ED-900 and isopropanol.

[0013] A preparation device for a block silicone oil softener comprises a tank body and a control panel, wherein a heating mechanism is embedded in the tank body, a stirring mechanism is arranged in the tank body, and a reflux reaction mechanism matching the stirring mechanism is arranged at the upper end of the tank body;

[0014] The number of the reflux reaction mechanisms is at least two and they are equidistantly arranged at the upper end of the tank body. The reflux reaction mechanism includes a traction component, a pumping component, a condenser and a coolant jacket. The pumping component is arranged at the upper end of the tank body, the traction component is arranged between the pumping component and the stirring mechanism, the condenser is arranged at the upper end of the tank body and is connected to the tank body to form a loop, and the coolant jacket is sheathed with the condenser and is connected to the pumping component.

[0015] The stirring mechanism includes a motor, a main shaft and a stirring blade. The motor is fixedly arranged at the upper end of the tank body, the main shaft is rotatably arranged in the tank body and is drivingly connected to the output shaft of the motor, the stirring blade is arranged on the main shaft and located in the tank body, and the traction assembly is arranged between the main shaft and the upper inner wall of the tank body.

[0016] The traction assembly includes a sealing cylinder, a synchronization head, a slide rail and a cable. The sealing cylinder is fixedly arranged on the upper inner wall of the tank body and is coaxially rotatably sealed with the main shaft. The slide rail is fixedly arranged in the sealing cylinder and is parallel to the length direction of the main shaft. The synchronization head is slidably connected to the slide rail. The main shaft is provided with a guide groove located in the sealing cylinder. The guide groove presents a sinusoidal structure when expanded. The synchronization head extends into the guide groove and is slidably connected thereto. One end of the cable is connected to the synchronization head, and the other end of the cable slides out of the sealing cylinder and is connected to the pumping assembly.

[0017] The pumping assembly includes a piston cylinder, a first plug body and a tension spring. The piston cylinder is integrally formed with the tank body. The first plug body is slidingly sealed in the piston cylinder. The tension spring is arranged at the upper end of the first plug body. The upper end of the piston cylinder is provided with a one-way liquid inlet and a one-way liquid outlet.

[0018] A one-way air inlet pipe and a one-way air exhaust pipe are provided at the lower end of the piston cylinder, and the one-way air exhaust pipe is connected to an air blowing pipe opening toward the condenser pipe.

[0019] A filtering mechanism is also provided between the lower side of the tank body and the main shaft, and the filtering mechanism includes a crank, a connecting rod, a pump fluid cylinder, a second plug body and a filter. The crank is fixedly connected to the lower end of the main shaft, the pump fluid cylinder is fixedly arranged in the tank body and a one-way liquid inlet valve is arranged on the upper side, the second plug body is slidingly sealed in the pump fluid cylinder, one end of the connecting rod is rotatably connected to the crank, and the other end of the connecting rod is hinged to the second plug body, the filter is arranged on the outside of the tank body, and the liquid inlet end is unidirectionally connected to the end of the pump fluid cylinder away from the connecting rod through a liquid pipe, and the liquid discharge end of the filter is unidirectionally connected to the tank body through a liquid pipe.

[0020] Compared with the prior art, the present invention has at least the following advantages:

[0021] The production method of the softener of the present application can improve production efficiency, and the block silicone oil softener can be produced with relatively simple production steps, thereby reducing production steps and processes and ensuring that the softener has good quality; by setting the reflux reaction mechanism, during the reflux reaction, the steam in the tank body can be effectively condensed to improve the reaction effect, and the stirring of the solvent can be synchronized with the pumping of the cooling liquid, and further, the steam in the tank body can be assisted to accelerate the flow to improve the efficiency and effect of condensation; the setting of the filtering mechanism can further cooperate with the stirring action to filter the impurities in the solvent to improve the purity of the solvent. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] The present invention is further illustrated by means of the non-limiting examples given in the accompanying drawings.

[0023] Figure 1 The present invention is a schematic structural diagram of a device for preparing a block silicone oil softener.

[0024] Figure 2 It is a structural cross-sectional view of the present invention.

[0025] Figure 3 for Figure 2 A magnified schematic diagram of center A.

[0026] Figure 4 It is a structural cross-sectional view from another angle of the present invention.

[0027] Figure 5 It is a structural schematic diagram of the stirring mechanism of the present invention.

[0028] Tank body 1, condenser 2, coolant jacket 21, motor 3, main shaft 31, stirring blade 32, sealing cylinder 4, synchronization head 41, cable 42, guide groove 43, piston cylinder 5, first plug body 51, tension spring 52, blowing pipe 6, crank 7, connecting rod 71, pump liquid cylinder 72, second plug body 73, filter 74. DETAILED DESCRIPTION

[0029] In order to enable those skilled in the art to better understand the present invention, the technical solution of the present invention is further described below in conjunction with the accompanying drawings and embodiments.

[0030] Example 1: Figure 1-5 As shown, a method for preparing a block silicone oil softener, the specific preparation steps are as follows:

[0031] Step 1: Prepare the epoxy-terminated double-capped end, any one of DMC or D4 and the catalyst required for the reaction;

[0032] Step 2: Add any one of the end epoxy double head, DMC or D4 and a catalyst into the tank body for reaction, wherein the reaction environment is heat preservation reaction and vacuumization, wherein the heating is continuously increased during the vacuuming process until the vacuum is completely obtained and then the heat is maintained to obtain the end epoxy silicone oil;

[0033] Step 3: Add the end epoxy silicone oil and the catalyst in step 2 into the tank body for reaction, wherein the reaction environment is a heat preservation reaction and a reflux reaction is carried out simultaneously, and finally the solvent is replaced to obtain the block silicone oil.

[0034] DMC is dimethyl carbonate, D4 ​​is octamethylcyclotetrasiloxane, and the catalyst includes dimethylacetamide, a base catalyst, polyetheramine ED-900 and isopropyl alcohol.

[0035] The catalysts used in step 2 and added before and after the processing sequence are dimethylacetamide and a base catalyst.

[0036] The catalysts used in step 3 and added in sequence are polyetheramine ED-900 and isopropyl alcohol.

[0037] A preparation device for a block silicone oil softener comprises a tank body 1 and a control panel, wherein a heating mechanism is embedded in the tank body 1, a stirring mechanism is arranged in the tank body 1, and a reflux reaction mechanism matching the stirring mechanism is arranged at the upper end of the tank body 1;

[0038] The number of reflux reaction mechanisms is at least two and they are equidistantly arranged at the upper end of the tank body 1. The reflux reaction mechanism includes a traction component, a pumping component, a condenser 2 and a cooling liquid jacket 21. The pumping component is arranged at the upper end of the tank body 1, the traction component is arranged between the pumping component and the stirring mechanism, the condenser 2 is arranged at the upper end of the tank body 1 and is connected to the tank body 1 to form a loop, and the cooling liquid jacket 21 is sleeved on the condenser 2 and is connected to the pumping component.

[0039] When preparing the softener, the existing epoxy end double-end caps on the market can be directly used, thereby reducing the production steps to improve the production efficiency and reduce the equipment required for preparing the pre-process. In the process of preparing the block silicone oil, the required solvent raw materials are added into the tank body 1, and the heating mechanism and the stirring mechanism are turned on through the control panel at the same time. The heating mechanism can heat the solvent to obtain the conditions required for the reflux reaction, and the stirring mechanism can mix and stir the solvent to improve the efficiency and effect of the reflux reaction.

[0040] When the solvent evaporates due to heating, the rising steam will gradually enter the condenser 2. At this time, the traction component will start the pumping component under the action of the stirring mechanism. The liquid inlet end of the pumping component is connected to the liquid outlet of the external coolant system. In this way, the pumping component will send the coolant into the coolant jacket 21, and the inlet into the coolant jacket 21 is the lowest level. In this way, the steam entering the condenser 2 is condensed under the action of the coolant in the coolant jacket 21 until it returns to the tank 1 in liquid form, so as to achieve full reaction of the solution and ensure the purity and quality of the production solution.

[0041] The stirring mechanism includes a motor 3, a main shaft 31 and a stirring blade 32. The motor 3 is fixedly arranged at the upper end of the tank body 1. The main shaft 31 is rotatably arranged in the tank body 1 and is drivingly connected to the output shaft of the motor 3. The stirring blade 32 is arranged on the main shaft 31 and is located in the tank body 1. The traction assembly is arranged between the main shaft 31 and the upper inner wall of the tank body 1.

[0042] The traction assembly includes a sealing cylinder 4, a synchronization head 41, a slide rail and a cable 42. The sealing cylinder 4 is fixedly arranged on the inner wall of the tank body 1 and is coaxially rotating and sealed with the main shaft 31. The slide rail is fixedly arranged in the sealing cylinder 4 and is parallel to the length direction of the main shaft 31. The synchronization head 41 is slidably connected to the slide rail. The main shaft 31 is provided with a guide groove 43 located in the sealing cylinder 4. The guide groove 43 presents a sinusoidal structure when unfolded. The synchronization head 41 extends into the guide groove 43 and is slidably connected thereto. One end of the cable 42 is connected to the synchronization head 41, and the other end of the cable 42 slides out of the sealing cylinder 4 and is connected to the pumping assembly.

[0043] The pumping assembly includes a piston cylinder 5, a first plug body 51 and a tension spring 52. The piston cylinder 5 is integrally formed with the tank body 1. The first plug body 51 is slidingly sealed in the piston cylinder 5. The tension spring 52 is arranged at the upper end of the first plug body 51. The upper end of the piston cylinder 5 is provided with a one-way liquid inlet and a one-way liquid outlet.

[0044] During stirring, the motor 3 starts to drive the main shaft 31 to rotate, and then the stirring blades 32 are used to mix and stir the solution in the tank body 1 to assist in promoting the reaction and mixing of the solvent. During the rotation of the main shaft 31, since the traction component is stationary relative to the main shaft 31, and the synchronous head 41 can only slide up and down through the guidance of the slide rail, under the guidance of the guide groove 43, the synchronous head 41 will synchronize with the rotation of the main shaft 31 to produce an up and down reciprocating circular motion. At this time, the synchronous head 41 will pull the first plug body 51 in the pumping component through the cable 42. When pulling and pulling, the first plug body 51 slides downward, and the negative pressure generated will draw the coolant in the external coolant system through the single-way liquid inlet. On the contrary, when the cable 42 cancels the traction of the first plug body 51, the coolant will be pumped into the coolant jacket 21 through the self-reset action of the tension spring 52, so as to achieve automatic circulation of the coolant, wherein the outlet of the coolant jacket 21 is the highest point of the level, which can ensure the effective circulation of the coolant.

[0045] Example 2: Figure 2 As shown, in a further improvement based on Example 1, a one-way air inlet pipe and a one-way air exhaust pipe are provided at the lower end of the piston cylinder 5, and the one-way air exhaust pipe is connected to a blowing pipe 6 opening toward the condenser 2.

[0046] In order to further improve the circulation efficiency and condensation effect of steam, the piston cylinder 5 and the tank body 1 can be sealed to form an independent space. When pumping coolant, the space under the first plug body 51 expands to generate negative pressure. At this time, the steam in the tank body 1 will be sucked into the one-way air inlet pipe. When sucking coolant, the space under the first plug body 51 is squeezed. At this time, the gas is squeezed and blown to the condenser 2 through the blowing pipe 6. According to the Bernoulli principle, the surrounding gas in the tank body 1 will be driven to accelerate the flow into the condenser 2, thereby actively gathering steam and accelerating the flow of gas, so as to promote the efficiency and effect of condensation, and be more conducive to solvent reaction.

[0047] Furthermore, a push-to-discharge valve is provided between the upper inner wall of the tank body 1 and the lower side of the piston cylinder 5. When the first plug body 51 moves downward to the lowest point, the push-to-discharge valve is squeezed, so that the lower side of the piston cylinder 5 opens to discharge part of the prematurely condensed solvent.

[0048] Example 3: Figure 1 and Figure 4 As shown, a further improvement on the basis of Example 1, a filtering mechanism is further provided between the lower side of the tank body 1 and the main shaft 31, the filtering mechanism comprising a crank 7, a connecting rod 71, a pump fluid cylinder 72, a second plug body 73 and a filter 74, the crank 7 is fixedly connected to the lower end of the main shaft 31, the pump fluid cylinder 72 is fixedly arranged in the tank body 1 and a one-way liquid inlet valve is provided on the upper side, the second plug body 73 is slidingly sealed and arranged in the pump fluid cylinder 72, one end of the connecting rod 71 is rotatably connected to the crank 7, and the other end of the connecting rod 71 is hinged to the second plug body 73, the filter 74 is arranged on the outside of the tank body 1 and the liquid inlet end is unidirectionally connected to the end of the pump fluid cylinder 72 away from the connecting rod 71 through a liquid pipe, and the liquid discharge end of the filter 74 is unidirectionally connected to the tank body 1 through a liquid pipe.

[0049] Furthermore, since epoxy bonds are easily destroyed under alkali catalysis and produce excessive impurities, during the reaction process, the filtering mechanism will circulate and filter the solvent to further improve the purity of the solvent. During filtering, the crank 7 synchronizes with the main shaft 31 to circulate, and the connecting rod 71 circulates and pulls the second plug body 73 in the pump cylinder 72. At this time, the pump cylinder 72 draws the solvent in the tank body 1 through the one-way liquid inlet valve, and then the second plug body 73 is pushed to squeeze the solvent, and finally transported through the liquid pipe and through the filter 74, and returned to the tank body 1 after filtration, thereby realizing automatic filtration of the solvent to improve the purity of the overall production.

[0050] The above embodiments are merely illustrative of the principles and effects of the present invention, and are not intended to limit the present invention. Anyone familiar with the technology may modify or change the above embodiments without violating the spirit and scope of the present invention. Therefore, all equivalent modifications or changes made by those with ordinary knowledge in the technical field without departing from the spirit and technical ideas disclosed by the present invention should still be covered by the claims of the present invention.

Claims

1. A preparation device for a block silicone oil softener, characterized in that: It comprises a tank body and a control panel, wherein a heating mechanism is embedded in the tank body, a stirring mechanism is arranged in the tank body, and a reflux reaction mechanism matching the stirring mechanism is arranged at the upper end of the tank body; The number of the reflux reaction mechanisms is at least two and they are equidistantly arranged at the upper end of the tank body. The reflux reaction mechanism comprises a traction assembly, a pumping assembly, a condenser and a cooling liquid jacket. The pumping assembly is arranged at the upper end of the tank body. The traction assembly is arranged between the pumping assembly and the stirring mechanism. The condenser is arranged at the upper end of the tank body and is connected to the tank body to form a loop. The cooling liquid jacket is sheathed with the condenser and is connected to the pumping assembly. The traction assembly includes a sealing cylinder, a synchronous head, a slide rail and a cable. The sealing cylinder is fixedly arranged on the upper inner wall of the tank body and is coaxially rotatably sealed with the main shaft. The slide rail is fixedly arranged in the sealing cylinder and is parallel to the length direction of the main shaft. The synchronous head is slidably connected with the slide rail. The main shaft is provided with a guide groove located in the sealing cylinder. The guide groove is a sinusoidal structure after being unfolded. The synchronous head extends into the guide groove and is slidably connected with the guide groove. One end of the cable is connected with the synchronous head, and the other end of the cable slides out of the sealing cylinder and is connected with the pumping assembly. The pumping assembly comprises a piston cylinder, a first plug body and a tension spring, the piston cylinder and the tank body are integrally formed, the first plug body is slidingly sealed in the piston cylinder, the tension spring is arranged at the upper end of the first plug body, and the upper end of the piston cylinder is provided with a one-way liquid inlet and a one-way liquid discharge port; A filtering mechanism is also provided between the lower side of the tank body and the main shaft, and the filtering mechanism includes a crank, a connecting rod, a pump fluid cylinder, a second plug body and a filter. The crank is fixedly connected to the lower end of the main shaft, the pump fluid cylinder is fixedly arranged in the tank body and a one-way liquid inlet valve is arranged on the upper side, the second plug body is slidingly sealed in the pump fluid cylinder, one end of the connecting rod is rotatably connected to the crank, and the other end of the connecting rod is hinged to the second plug body, the filter is arranged on the outside of the tank body, and the liquid inlet end is unidirectionally connected to the end of the pump fluid cylinder away from the connecting rod through a liquid pipe, and the liquid discharge end of the filter is unidirectionally connected to the tank body through a liquid pipe.

2. The preparation equipment of a block silicone oil softener according to claim 1, characterized in that: The stirring mechanism includes a motor, a main shaft and a stirring blade. The motor is fixedly arranged at the upper end of the tank body, the main shaft is rotatably arranged in the tank body and is drivingly connected to the output shaft of the motor, the stirring blade is arranged on the main shaft and located in the tank body, and the traction assembly is arranged between the main shaft and the upper inner wall of the tank body.

3. The preparation equipment of a block silicone oil softener according to claim 2, characterized in that: A one-way air inlet pipe and a one-way air exhaust pipe are provided at the lower end of the piston cylinder, and the one-way air exhaust pipe is connected to an air blowing pipe opening toward the condenser pipe.

4. A method for preparing a block silicone oil softener, characterized in that: The preparation is carried out using the preparation equipment described in any one of claims 1 to 3, and the specific preparation steps are as follows: Step 1: prepare the terminal epoxy double cap, any one of DMC or D4 and the catalyst required for the reaction, wherein the DMC is dimethyl carbonate, the D4 is octamethylcyclotetrasiloxane, and the catalyst includes dimethylacetamide, a base catalyst, polyetheramine ED-900 and isopropyl alcohol; Step 2: Add any one of the end epoxy double head, DMC or D4 and a catalyst into the tank body for reaction, wherein the reaction environment is heat preservation reaction and vacuumization, wherein the heating is continuously increased during the vacuuming process until the vacuum is completely obtained and then the heat is maintained to obtain the end epoxy silicone oil; Step 3: Add the end epoxy silicone oil and the catalyst in step 2 into the tank body for reaction, wherein the reaction environment is a heat preservation reaction and a reflux reaction is carried out simultaneously, and finally the solvent is replaced to obtain the block silicone oil.

5. The method for preparing a block silicone oil softener according to claim 4, characterized in that: The catalysts used in step 2 and added in sequence are dimethylacetamide and a base catalyst.

6. The method for preparing a block silicone oil softener according to claim 5, characterized in that: The catalysts used in step 3 and added in sequence are polyetheramine ED-900 and isopropanol.

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