Organic heat carrier flash point improver and preparation method and device thereof

Abstract

The invention discloses an organic heat carrier flash point improver and a preparation method and device thereof, and relates to the technical field of organic heat carriers. The graphene oxide modified ammonium polyphosphate lubricating oil is prepared from the following components: high-flash-point solvent oil, graphene oxide modified ammonium polyphosphate, an antioxidant, a flocculating agent and N, N '-di-salicylidene propylene diamine. According to the organic heat carrier flash point improver disclosed by the invention, the metal deactivator, the antioxidant and the flocculant are compounded by adopting a method of mixing the graphene oxide modified ammonium polyphosphate and the high-flash-point solvent oil, so that the dispersion uniformity and stability of graphene in heat-conducting oil can be effectively improved, and the heat conduction efficiency of the heat-conducting oil is effectively improved; aging coking and flash point reduction caused by local overheating of the heat-conducting oil in the using process are prevented, the using performance of the heat-conducting oil is effectively improved, and the flash point is increased by 5-9%; the preparation method of the organic heat carrier flash point improver is simple and easy to operate. In the using process, the heat-conducting oil additive can be directly added into heat-conducting oil, is safe and rapid, and is suitable for industrial application.

Description

Technical Field

[0001] The invention relates to the technical field of organic heat carriers, in particular to an organic heat carrier flash point improver and a preparation method and device thereof. Background Art

[0002] The flash point of an organic heat carrier refers to the lowest temperature at which a mixture of vapor volatilized from the surface of the organic heat carrier and air can flash instantly when encountering a fire source under specified test conditions. The flash point is one of the important indicators for measuring the safety performance of organic heat carriers. The higher the flash point, the better the safety of the organic heat carrier at high temperatures. During the use of organic heat carriers, due to high-temperature operation and cracking and oxidation, the flash point will gradually decrease, posing a safety hazard.

[0003] In order to solve this problem, the existing technology uses an organic heat carrier filtration dehydrogenation device and regular inspection and maintenance. Using an organic heat carrier filtration dehydrogenation device, this device can separate the low components and hydrogen components in the organic heat carrier through a purification and filtration process and use negative pressure vacuum supporting equipment, thereby improving the flash point and initial distillation point of the organic heat carrier. In addition, regular inspection of various indicators of the organic heat carrier is also an important measure to prevent the flash point from decreasing. When the organic heat carrier operates in a high temperature and closed environment in the system for a long time, cracking and deterioration will occur, resulting in problems such as reduced flash point, increased acid value, and increased residual carbon. If other indicators are normal, the flash point can be repaired by replacing part of the organic heat carrier, but this is only a temporary solution, so it is necessary to regularly inspect and record data. Although the above method can improve the flash point problem of the organic heat carrier and ensure its safety and stability during use, it also has problems such as the need for special equipment and a large amount of manpower maintenance.

[0004] Therefore, in view of the physical and chemical properties of organic heat carriers and the current status of their application and flash point improvement, it is very necessary to design an organic heat carrier flash point improver and its preparation method which can effectively improve the flash point of organic heat carriers, improve the quality of organic heat carriers, realize online improvement of organic heat carriers in organic heat carrier circulation systems, improve production efficiency, and reduce environmental pollution. Summary of the invention

[0005] The purpose of the present invention is to provide an organic heat carrier flash point improver and a preparation method and device thereof in order to solve the problems existing in the background technology.

[0006] To achieve the above object, the present invention provides the following technical solutions: The first technical purpose of the present invention is to provide an organic heat carrier flash point improver, which is prepared from the following components in parts by weight: 50-85 parts of high flash point solvent oil; 5-25 parts of graphene oxide modified ammonium polyphosphate; 2-10 parts of antioxidant; 2 to 10 parts of flocculant; 1 to 5 parts of N,N'-disalicylidenepropylenediamine

[0007] The graphene oxide modified ammonium polyphosphate is prepared by the following method: S1: First, crush the ammonium polyphosphate to a particle size of 100-200 meshes, mix the crushed ammonium polyphosphate and the silane coupling agent γ-aminopropyltriethoxysilane evenly according to the molar ratio of γ-aminopropyltriethoxysilane: ammonium polyphosphate = 1:5-20, and then disperse them in 50% ethanol according to the mass ratio of γ-aminopropyltriethoxysilane: ethanol = 1:1-1.5, react at 90-110°C for 3-5 hours, and set aside; S2: adding a graphene oxide solution with a concentration of 20 g / l into an anhydrous ethanol solution to prepare a dispersion, wherein the volume ratio of the graphene oxide solution to the anhydrous ethanol solution is 1:5-10, and the weight of the graphene oxide in the dispersion accounts for 0.01-0.1 wt.% of the total weight of the dispersion, and the dispersion is ultrasonically enhanced dispersed for standby use; S3: adding the dispersion prepared in step S2 to the dispersion prepared in step S1 at a molar ratio of ammonium polyphosphate to graphene oxide of 1:10-25, and continuing the reaction at 90-110° C. for 3-5 h to obtain a gray-black solid for standby use; S4: Grinding the material to a particle size of 500-900 mesh using a ball mill according to a ratio of material to ball milling medium = 1:3, washing with deionized water for 3-5 times, and freeze-drying to obtain the graphene oxide modified ammonium polyphosphate, wherein the ball milling medium is one or a mixture of water, alcohol, toluene or tetrahydrofuran.

[0008] Preferably, the high flash point solvent oil is an aromatic solvent oil having a flash point greater than 100° C. as measured by a closed cup method.

[0009] Preferably, the antioxidant is any one of isooctyl propionate, p-phenylenediamine, and dihydroquinoline.

[0010] Preferably, the flocculant is any one of polyacrylate and polymethacrylate.

[0011] The second technical purpose of the present invention is to provide a preparation and production process of an organic heat carrier flash point improver, comprising the following steps: Step 1: Preparation of graphene oxide modified ammonium polyphosphate.

[0012] Step 2: Add the graphene oxide modified ammonium polyphosphate and N,N'-disalicylidene propylene diamine prepared in step 1 in a certain proportion to the high flash point solvent oil, heat to 60-120°C, and stir for 10-60 min. Continue to add the antioxidant and flocculant in a certain proportion, stir for 30-90 minutes, and obtain the organic heat carrier flash point improver.

[0013] Another object of the present invention is to provide a production equipment for preparing the organic heat carrier flash point improver. The ball mill used in step S4 includes a base, the top of the base is rotatably connected to a rotating frame, the outer wall of the rotating frame is rotatably connected to a rotating cylinder, the outer wall of the rotating cylinder is fixedly connected to a gear ring, a first motor is provided at the top of the base, the output end of the first motor is connected to a first spur gear, the first spur gear is in contact with the gear ring, the first spur gear is meshed with the gear ring, the rotating cylinder crushes the material through a crushing mechanism, and the rotating cylinder performs a discharging operation through a discharging mechanism.

[0014] As a further solution of the present invention: the crushing mechanism includes a first transverse plate, which is fixedly connected to the inner wall of the rotating cylinder at equal intervals in a circumference, a push plate is slidably connected to one end of the inner wall of the rotating cylinder, a grid cylinder is fixedly connected to the outer wall of the push plate, and a second transverse plate is fixedly connected to the inner wall of the grid cylinder at equal intervals in a circumference, an annular cover is provided at one end of the rotating cylinder, a baffle is provided in the inner cavity of the annular cover, a through hole is opened on the outer wall of the annular cover, a mounting hole is opened at the position where the outer wall of the rotating cylinder and the through hole meet, a bolt is threadedly connected to the inner wall of the mounting hole, a slot is symmetrically opened on the outer wall of the grid cylinder up and down, a fixing groove is symmetrically opened on the inner wall of the annular cover up and down, a rotating column is rotatably connected to the outer wall of one end of the baffle, and a first bevel gear is fixedly connected to one end of the rotating column, the inner wall of the baffle is located inside the first bevel gear and is rotatably connected to the second bevel gear, the inner wall of the second bevel gear is fixedly connected to a first threaded rod, and fixed blocks are connected at both ends of the first threaded rod, and the fixed block is slidably connected to the inside of the baffle and extends out of the baffle.

[0015] As a further solution of the present invention: the discharging mechanism includes a connecting column, which is fixedly connected to one end of the rotating cylinder, a displacement rod extending to the bottom end of the connecting column is slidably connected inside the base, a second motor is installed on one side of the displacement rod at the top of the base, and a second threaded rod is connected to the output end of the second motor, a second spur gear is rotatably connected to the outer wall of the displacement rod inside the base, a displacement seat is slidably connected to the outer wall of the second spur gear inside the base, the first spur gear is installed at the top of the displacement seat, and a third spur gear is rotatably connected to the lower part of the first spur gear inside the base, a rotating disk is fixedly connected to one end of the base, a groove is provided at one end of the base, a limiting column is fixedly connected to the inner wall of the groove, a shaking seat is slidably connected to the outer wall of the limiting column, a collecting seat is provided in the inner cavity of the shaking seat, a placing seat is provided at the top of the collecting seat, a sliding rod is fixedly connected to one end of the rotating disk, a sliding groove is provided on the outer wall of the shaking seat, and a grid plate is fixedly connected to the inner wall of the placing seat.

[0016] As a further solution of the present invention: the inner walls of the slot and the fixing slot are fitted with the outer wall of the fixing block, the first bevel gear is meshed with the second bevel gear, the outer wall of the first threaded rod is symmetrically provided with external threads, the inner wall of the fixing block is provided with a first threaded hole, and the external thread matches the first threaded hole.

[0017] As a further solution of the present invention: the outer walls of the displacement rod and the displacement seat are both provided with tooth grooves, the tooth grooves are meshed with the second spur gear, the outer wall of the displacement rod is provided with a second threaded hole, the second threaded hole matches the second threaded rod, the first spur gear is meshed with the third spur gear, the outer wall of the sliding rod is fitted with the inner wall of the sliding groove, the outer wall of the rocking seat is provided with a limiting hole, and the inner wall of the limiting hole is fitted with the outer wall of the limiting column.

[0018] As a further solution of the present invention: a guide column extending into the interior of the displacement seat is fixedly connected to the interior of the base, a guide groove is provided at the bottom end of the displacement seat, an outer wall of the guide column is fitted with an inner wall of the guide groove, and the outer wall of the guide column is square in shape.

[0019] Compared with the prior art, the present invention has the following beneficial effects: 1. The flash point improver of the organic heat carrier of the present invention adopts the method of mixing graphene oxide modified ammonium polyphosphate with high flash point solvent oil, compounding metal passivator, antioxidant and flocculant, which can effectively improve the uniformity and stability of graphene dispersion in heat transfer oil, effectively improve the heat transfer efficiency of heat transfer oil, prevent local overheating of heat transfer oil during use, delay aging and coking of heat transfer oil, effectively improve the use performance of heat transfer oil, and increase the flash point by 5-9%; 2. The preparation method of the organic heat carrier flash point improver of the present invention is simple and easy to operate. It can be directly added to the heat transfer oil during use, which is safe and fast and suitable for industrial application; 3. By setting up a crushing mechanism, steel balls are set in both the rotating cylinder and the grid cylinder. The diameter of the steel balls in the rotating cylinder is smaller than that of the steel balls in the grid cylinder. When the material is put into the grid cylinder, the grid cylinder rotates and drives the steel balls to impact and crush the material. After the material is initially crushed, the material falls into the rotating cylinder through the holes on the grid cylinder. The steel balls in the rotating cylinder then perform ball milling on the material, which is convenient for fully ball milling the material and improves the effect of ball milling. 4. By setting up the discharging mechanism, the second motor drives the displacement rod to move, and the displacement of the displacement rod drives the rotating cylinder to rotate through the connecting column, and the material and steel balls in the rotating cylinder are poured into the placement seat. At the same time, the movement of the displacement rod drives the first spur gear to move and contact with the third spur gear. Then the first motor can be started to drive the rotating disk to rotate. The rotation of the rotating disk drives the shaking seat to reciprocate on the outer wall of the limiting column through the sliding rod. The shaking seat moves to shake the collecting seat and the placing seat, and the material in the placing seat falls into the collecting seat through the grid plate for collection operation, which is convenient for discharging the rotating cylinder and automatically separating the steel balls and materials. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a structural schematic diagram of the present invention; Figure 2 is a cross-sectional view of a rotating drum of the present invention; Figure 3 It is a schematic diagram of the installation of the annular cover of the present invention; Figure 4 is a cross-sectional view of a baffle of the present invention; Figure 5 is a cross-sectional view of a base of the present invention; Figure 6 It is a schematic diagram of the installation of the rocking seat of the present invention; Figure 7 It is a structural schematic diagram of the slide bar of the present invention; Figure 8 It is a cross-sectional view of the collecting seat and the placing seat of the present invention.

[0021] In the figure: 1, base; 2, rotating frame; 3, rotating cylinder; 4, gear ring; 5, first motor; 6, first straight gear; 7, crushing mechanism; 701, first horizontal plate; 702, push plate; 703, grid cylinder; 704, second horizontal plate; 705, annular cover; 706, through hole; 707, mounting hole; 708, bolt; 709, baffle; 710, slot; 711, fixing slot; 712, rotating column; 713, first bevel gear; 714, second bevel gear; 715, The first threaded rod; 716, fixed block; 8, discharging mechanism; 801, connecting column; 802, displacement rod; 803, second threaded rod; 804, second motor; 805, second spur gear; 806, displacement seat; 807, third spur gear; 808, rotating disk; 809, groove; 810, shaking seat; 811, limiting column; 812, collecting seat; 813, placing seat; 814, sliding rod; 815, sliding groove; 816, grid plate; 9, guide column; 10, guide groove. DETAILED DESCRIPTION

[0022] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, which are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance. In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected", and "set" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or it can be the internal connection of two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. The following is an explanation of an embodiment of the present invention based on the overall structure of the present invention.

[0024] Example 1 Preparation of an organic heat carrier flash point improver See also Figures 1 to 8In an embodiment of the present invention, an organic heat carrier flash point improver is prepared from the following components in parts by weight: 50 parts of high flash point solvent oil; 15 parts of graphene oxide modified ammonium polyphosphate; 2 parts of 2-ethylhexyl propionate; Polyacrylate 2 parts; 1 part of N,N'-disalicylidenepropylenediamine.

[0025] High flash point solvent oil is an aromatic solvent oil with a flash point greater than 100°C measured by the closed cup method.

[0026] The preparation method of an organic heat carrier flash point improver comprises the following steps: Step 1: Preparation of graphene oxide modified ammonium polyphosphate: S1: First, crush the ammonium polyphosphate to a particle size of 100 mesh, mix the crushed ammonium polyphosphate and the silane coupling agent γ-aminopropyl triethoxysilane evenly according to the molar ratio of γ-aminopropyl triethoxysilane: ammonium polyphosphate = 1:50, and then disperse them in 50% ethanol according to the mass ratio of γ-aminopropyl triethoxysilane: ethanol = 1:1, react at 90°C for 5 h, and set aside; S2: adding a graphene oxide solution with a concentration of 20 g / l into an anhydrous ethanol solution to prepare a dispersion, wherein the volume ratio of the graphene oxide solution to the anhydrous ethanol solution is 1:5, and the weight of the graphene oxide in the dispersion accounts for 0.1 wt.% of the total weight of the dispersion, and the dispersion is ultrasonically enhanced dispersed for later use; S3: adding the dispersion prepared in step S2 to the dispersion prepared in step S1 at a molar ratio of ammonium polyphosphate to graphene oxide of 1:10, and continuing the reaction at 90° C. for 5 h to obtain a gray-black solid for standby use; S4: Grinding the material to a particle size of 500-900 meshes using a ball mill according to a ratio of material to ball milling medium = 1:3, washing with deionized water for 3-5 times, and freeze-drying to obtain graphene oxide modified ammonium polyphosphate, wherein the ball milling medium is one or a mixture of water, alcohol, toluene or tetrahydrofuran.

[0027] Step 2: Add the graphene oxide modified ammonium polyphosphate and N,N'-disalicylidenepropylenediamine prepared in step 1 in a certain proportion to high flash point solvent oil in sequence, heat to 60-120°C, stir for 10-60 min, continue to add the antioxidant and flocculant in a certain proportion, stir for 30-90 minutes, and obtain an organic heat carrier flash point improver.

[0028] A preparation device for preparing an organic heat carrier flash point improver, the ball mill used in step S4 includes a base 1, the top of the base 1 is rotatably connected to a rotating frame 2, the outer wall of the rotating frame 2 is rotatably connected to a rotating cylinder 3, the outer wall of the rotating cylinder 3 is fixedly connected to a gear ring 4, a first motor 5 is arranged at the top of the base 1, the output end of the first motor 5 is connected to a first spur gear 6, the first spur gear 6 is in contact with the gear ring 4, the first spur gear 6 is meshed with the gear ring 4, the rotating cylinder 3 performs a material crushing operation through a crushing mechanism 7, the rotating cylinder 3 performs a material discharging operation through a discharging mechanism 8, the crushing mechanism 7 includes a first transverse plate 701, the first transverse plate 701 is fixedly connected to the inner wall of the rotating cylinder 3 at equal distances around the circumference, one end of the inner wall of the rotating cylinder 3 is slidably connected to a push plate 702, the outer wall of the push plate 702 is fixedly connected to a grid cylinder 703, the inner wall of the grid cylinder 703 is fixedly connected to a second transverse plate 704 at equal distances around the circumference, the rotating cylinder 3 is fixedly connected to the outer wall of the grid cylinder 703, and the rotating cylinder 3 is fixedly connected to the outer wall of the grid cylinder 703. An annular cover 705 is provided at one end of the moving cylinder 3, and a baffle 709 is provided in the inner cavity of the annular cover 705. A through hole 706 is provided on the outer wall of the annular cover 705. A mounting hole 707 is provided at the position where the outer wall of the rotating cylinder 3 and the through hole 706 meet. A bolt 708 is threadedly connected to the inner wall of the mounting hole 707. Slots 710 are symmetrically provided on the outer wall of the grid cylinder 703, and fixing grooves 711 are symmetrically provided on the inner wall of the annular cover 705. A rotating column 712 is rotatably connected to the outer wall of one end of the baffle 709, and a first bevel gear 713 is fixedly connected to one end of the rotating column 712. The inner wall of the baffle 709 is located inside the first bevel gear 713 and is rotatably connected to the outer wall of the second bevel gear 714. The inner wall of the second bevel gear 714 is fixedly connected to a first threaded rod 715. Fixed blocks 716 are connected to both ends of the first threaded rod 715. The fixed block 716 is slidably connected to the inside of the baffle 709 and extends out of the baffle 709.

[0029] In this embodiment: the first motor 5 is started, and the first motor 5 drives the first spur gear 6 to rotate, the first spur gear 6 rotates to drive the gear ring 4 to rotate, the gear ring 4 rotates to drive the rotating cylinder 3 to rotate, the rotating cylinder 3 rotates through the push plate 702 to drive the grid cylinder 703 to rotate, and when ball milling is performed, steel balls are arranged in the rotating cylinder 3 and the grid cylinder 703, and the diameter of the steel balls in the rotating cylinder 3 is smaller than the diameter of the steel balls in the grid cylinder 703, and the material is put into the grid cylinder 703, and the grid cylinder 703 rotates to drive the steel balls to impact and crush the material, and after the material is initially crushed, the material falls into the rotating cylinder 3 through the holes on the grid cylinder 703, and the steel balls in the rotating cylinder 3 perform a ball milling operation on the material, which is convenient for fully ball milling the material and improves the effect of ball milling; When installing the device, the push plate 702 is moved to one end of the rotating cylinder 3 so that the grid cylinder 703 enters the rotating cylinder 3, and then the steel balls are respectively placed in the rotating cylinder 3 and the grid cylinder 703, and the annular cover 705 is connected to one end of the rotating cylinder 3, and the annular cover 705 is sleeved on the outer wall of the grid cylinder 703, and the bolt 708 is connected through the through hole 706 and enters the mounting hole 707 to fix the annular cover 705; then the baffle 709 is connected to the inner wall of the annular cover 705, and the rotating column 712 is rotated. The rotation of the rotating column 712 drives the first bevel gear 713 to rotate, and the rotation of the first bevel gear 713 drives the second bevel gear 714 to rotate, and the rotation of the second bevel gear 714 drives the first threaded rod 715 to rotate, and the rotation of the first threaded rod 715 drives the fixed block 716 to move, and the fixed block 716 moves through the slot 710 and moves into the fixed groove 711, thereby fixing the baffle 709; When taking out the material in the rotating cylinder 3, first open the baffle 709 so that the steel balls in the grid cylinder 703 can be directly taken out first, then remove the annular cover 705, move the material and the steel balls out from one end of the rotating cylinder 3, and at the same time, the movable grid cylinder 703 drives the push plate 702 to move, and the push plate 702 moves to scrape out the residual material in the rotating cylinder 3.

[0030] Please refer to Figures 5 to 8 The discharging mechanism 8 includes a connecting column 801, which is fixedly connected to one end of the rotating cylinder 3. A displacement rod 802 extending to the bottom end of the connecting column 801 is slidably connected inside the base 1. A second motor 804 is installed on one side of the displacement rod 802 at the top of the base 1. A second threaded rod 803 is connected to the output end of the second motor 804. A second spur gear 805 is rotatably connected to the outer wall of the displacement rod 802 inside the base 1. A displacement seat 806 is slidably connected to the outer wall of the second spur gear 805 inside the base 1. The first motor 5 is installed on the top of the displacement seat 806. The inside of the base 1 A third spur gear 807 is rotatably connected to the lower portion of the first spur gear 6, one end of the third spur gear 807 is fixedly connected to a rotating disk 808, one end of the base 1 is provided with a groove 809, the inner wall of the groove 809 is fixedly connected to a limiting column 811, the outer wall of the limiting column 811 is slidably connected to a rocking seat 810, the inner cavity of the rocking seat 810 is provided with a collecting seat 812, the top of the collecting seat 812 is provided with a placing seat 813, one end of the rotating disk 808 is fixedly connected to a sliding rod 814, the outer wall of the rocking seat 810 is provided with a sliding groove 815, and the inner wall of the placing seat 813 is fixedly connected to a grid plate 816.

[0031] In this embodiment: when the material is discharged, the second motor 804 is started, and the second motor 804 drives the second threaded rod 803 to rotate, and the second threaded rod 803 rotates to drive the displacement rod 802 to move, and the displacement rod 802 moves through the connecting column 801 to drive the rotating cylinder 3 to rotate, and the material and steel balls in the rotating cylinder 3 are poured into the placement seat 813 and located at the top of the grid plate 816, and at the same time, the displacement rod 802 moves to drive the second spur gear 805 to rotate, and the second spur gear 805 rotates to drive the displacement seat 806 to move, and the displacement seat 806 moves to drive the first spur gear 6 to move with the third spur gear 813. Gears 807 are in contact, and then the first motor 5 can be started to drive the first spur gear 6 to rotate. The rotation of the first spur gear 6 drives the third spur gear 807 to rotate. The rotation of the third spur gear 807 drives the rotating disk 808 to rotate. The rotating disk 808 rotates through the sliding rod 814 to drive the shaking seat 810 to reciprocate on the outer wall of the limiting column 811. The shaking seat 810 moves to shake the collecting seat 812 and the placing seat 813. The material in the placing seat 813 falls into the collecting seat 812 through the mesh plate 816 for collection operation, which is convenient for discharging the rotating cylinder 3 and automatically separating the steel balls and materials.

[0032] Please refer to Figures 1 to 4 The inner walls of the slot 710 and the fixing slot 711 fit with the outer wall of the fixing block 716, the first bevel gear 713 meshes with the second bevel gear 714, the outer wall of the first threaded rod 715 is symmetrically provided with external threads, and the inner wall of the fixing block 716 is provided with a first threaded hole, and the external thread matches the first threaded hole.

[0033] In this embodiment: the annular cover 705 is connected to one end of the rotating cylinder 3, the annular cover 705 is sleeved on the outer wall of the grid cylinder 703, and the bolt 708 is connected through the through hole 706 and connected into the mounting hole 707 to fix the annular cover 705; then the baffle 709 is connected to the inner wall of the annular cover 705, and the rotating column 712 is rotated. The rotation of the rotating column 712 drives the first bevel gear 713 to rotate, and the rotation of the first bevel gear 713 drives the second bevel gear 714 to rotate. The rotation of the second bevel gear 714 drives the first threaded rod 715 to rotate, and the rotation of the first threaded rod 715 drives the fixing block 716 to move, and the fixing block 716 moves through the slot 710 and moves into the fixing groove 711, thereby fixing the baffle 709.

[0034] Please refer to Figures 5 to 8The outer walls of the displacement rod 802 and the displacement seat 806 are both provided with tooth grooves, which mesh with the second spur gear 805. The outer wall of the displacement rod 802 is provided with a second threaded hole, which matches the second threaded rod 803. The first spur gear 6 meshes with the third spur gear 807. The outer wall of the sliding rod 814 fits with the inner wall of the sliding groove 815. The outer wall of the rocking seat 810 is provided with a limiting hole, and the inner wall of the limiting hole fits with the outer wall of the limiting column 811.

[0035] In this embodiment: the second motor 804 drives the second threaded rod 803 to rotate, the rotation of the second threaded rod 803 drives the displacement rod 802 to move, the movement of the displacement rod 802 drives the second spur gear 805 to rotate, the rotation of the second spur gear 805 drives the displacement seat 806 to move, the displacement of the displacement seat 806 drives the first spur gear 6 to move and contact with the third spur gear 807, the first motor 5 drives the rotating disk 808 to rotate, the rotation of the rotating disk 808 drives the shaking seat 810 to reciprocate on the outer wall of the limiting column 811 through the sliding rod 814.

[0036] Please refer to Figures 5 to 8 The base 1 is fixedly connected to a guide column 9 extending into the displacement seat 806. The bottom end of the displacement seat 806 is provided with a guide groove 10. The outer wall of the guide column 9 fits with the inner wall of the guide groove 10, and the outer wall of the guide column 9 is square in shape.

[0037] In this embodiment, when the displacement seat 806 moves, the guide column 9 slides in the guide groove 10 to limit the displacement direction of the displacement seat 806 .

[0038] Example 2 Preparation of an organic heat carrier flash point improver An organic heat carrier flash point improver is prepared from the following components in parts by weight: 70 parts of high flash point solvent oil; 5 parts of graphene oxide modified ammonium polyphosphate; 6 parts of p-phenylenediamine; 6 parts of polymethacrylate; 3 parts of N,N'-disalicylidenepropylenediamine.

[0039] High flash point solvent oil is an aromatic solvent oil with a flash point greater than 100°C measured by the closed cup method.

[0040] The preparation method of an organic heat carrier flash point improver comprises the following steps: Step 1: Preparation of graphene oxide modified ammonium polyphosphate: S1: First, crush the ammonium polyphosphate to a particle size of 150 mesh, mix it evenly according to the molar ratio of silane coupling agent γ-aminopropyltriethoxysilane: ammonium polyphosphate = 1:15, and then disperse it in 50% ethanol according to the mass ratio of γ-aminopropyltriethoxysilane: ethanol = 1:1.3, react at 100°C for 4 h, and set aside; S2: adding a graphene oxide solution with a concentration of 20 g / l into an anhydrous ethanol solution to prepare a dispersion, wherein the volume ratio of the graphene oxide solution to the anhydrous ethanol solution is 1:8, and the weight of the graphene oxide in the dispersion accounts for 0.05 t.% of the total weight of the dispersion, and the dispersion is ultrasonically enhanced dispersed for standby use; S3: adding the dispersion prepared in step S2 to the dispersion prepared in step S1 at a molar ratio of ammonium polyphosphate to graphene oxide of 1:15, and continuing the reaction at 100° C. for 4 h to obtain a gray-black solid for standby use; S4: Grinding the material to a particle size of 500-900 meshes using a ball mill according to a ratio of material to ball milling medium = 1:3, washing with deionized water for 3-5 times, and freeze-drying to obtain graphene oxide modified ammonium polyphosphate. The ball milling medium is one or a mixture of water, alcohol, toluene or tetrahydrofuran.

[0041] Step 2: Add the graphene oxide modified ammonium polyphosphate and N,N'-disalicylidene propylene diamine prepared in step 1 in a certain proportion to high flash point solvent oil in sequence, heat to 60-120° C., stir for 10-60 min, continue to add a certain proportion of antioxidant and flocculant, stir for 30-90 minutes, and obtain an organic heat carrier flash point improver; The application equipment is the same as that in Example 1 and will not be described in detail here.

[0042] Example 3 An organic heat carrier flash point improver is prepared from the following components in parts by weight: 85 parts of high flash point solvent oil; Graphene oxide modified ammonium polyphosphate 25 parts; 10 parts of dihydroquinoline; 10 parts of polymethacrylate; 5 parts of N,N'-disalicylidenepropylenediamine.

[0043] High flash point solvent oil is an aromatic solvent oil with a flash point greater than 100°C measured by the closed cup method.

[0044] The preparation method of an organic heat carrier flash point improver comprises the following steps: Step 1: Preparation of graphene oxide modified ammonium polyphosphate: S1: First, crush the ammonium polyphosphate to a particle size of 200 mesh, mix the silane coupling agent γ-aminopropyltriethoxysilane and ammonium polyphosphate in a molar ratio of 1:20, and then disperse it in 50% ethanol in a mass ratio of γ-aminopropyltriethoxysilane and ethanol in a mass ratio of 1:1.5, react at 110°C for 5 h, and set aside; S2: adding a graphene oxide solution having a concentration of 20 g / l into an anhydrous ethanol solution to prepare a dispersion, wherein the volume ratio of the graphene oxide solution to the anhydrous ethanol solution is 1:10, and the weight of the graphene oxide in the dispersion accounts for 0.01 wt.% of the total weight of the dispersion, and the dispersion is ultrasonically enhanced dispersed for later use; S3: adding the dispersion prepared in step S2 to the dispersion prepared in step S1 at a molar ratio of ammonium polyphosphate to graphene oxide of 1:25, and continuing the reaction at 110° C. for 5 h to obtain a gray-black solid for standby use; S4: Grinding the material to a particle size of 500-900 meshes using a ball mill according to a ratio of material to ball milling medium = 1:3, washing with deionized water for 3-5 times, and freeze-drying to obtain graphene oxide modified ammonium polyphosphate. The ball milling medium is one or a mixture of water, alcohol, toluene or tetrahydrofuran.

[0045] Step 2: Add the graphene oxide modified ammonium polyphosphate and N,N'-disalicylidene propylene diamine prepared in step 1 in a certain proportion to the high flash point solvent oil, heat to 60-120°C, and stir for 10-60 min. Continue to add the antioxidant and flocculant in a certain proportion, stir for 30-90 minutes, and obtain the organic heat carrier flash point improver.

[0046] The application equipment is the same as that in Example 1 and will not be described in detail here.

[0047] Comparative Example 1 Preparation of an organic heat carrier flash point improver, the specific implementation method is the same as Example 2, the only difference is that graphene oxide modified ammonium polyphosphate is not added.

[0048] Comparative Example 2 Preparation of an organic heat carrier flash point improver, the specific implementation method is the same as Example 2, the only difference is that the antioxidant p-phenylenediamine is not added.

[0049] Performance Testing: The flash point improvers prepared in the above-mentioned embodiments and comparative examples were respectively added to the organic heat carrier circulation system; the organic heat carrier circulation system was heated to maintain a temperature of 200° C. to 270° C., and the heating operation was continued for 15 to 30 days.

[0050] The observation results of the comparative experiment are shown in the following table.

[0051]

[0052] The flash point improver of the organic heat carrier of the present invention can effectively improve the flash point by 5% to 9%, and the kinematic viscosity and filter paper weight gain tests are better than the existing comparative examples. It can improve the antioxidant performance of the organic heat carrier in use, delay or prevent the oxidation and flash point reduction of the organic heat carrier, significantly improve the thermal conductivity, and significantly improve the flash point before and after use.

[0053] What is described above is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. An organic heat carrier flash point improver, characterized in that: Made from the following components in parts by weight: 50-85 parts of high flash point solvent oil; 5-25 parts of graphene oxide modified ammonium polyphosphate; 2-10 parts of antioxidant; 2 to 10 parts of flocculant; 1 to 5 parts of N,N'-disalicylidenepropylenediamine 2. An organic heat carrier flash point improver according to claim 1, characterized in that: The preparation steps of the graphene oxide modified ammonium polyphosphate are as follows: S1: First, crush the ammonium polyphosphate to a particle size of 100-200 meshes, mix the crushed ammonium polyphosphate and the silane coupling agent γ-aminopropyltriethoxysilane evenly according to the molar ratio of γ-aminopropyltriethoxysilane: ammonium polyphosphate = 1:5-20, and then disperse them in 50% ethanol according to the mass ratio of γ-aminopropyltriethoxysilane: ethanol = 1:1-1.5, react at 90-110°C for 3-5 hours, and set aside; S2: adding a graphene oxide solution with a concentration of 20 g / l into an anhydrous ethanol solution to prepare a dispersion, wherein the volume ratio of the graphene oxide solution to the anhydrous ethanol solution is 1:5-10, and the weight of the graphene oxide in the dispersion accounts for 0.01-0.1 wt.% of the total weight of the dispersion, and the dispersion is ultrasonically enhanced dispersed for standby use; S3: adding the dispersion prepared in step S2 to the dispersion prepared in step S1 at a molar ratio of ammonium polyphosphate to graphene oxide of 1:10-25, and continuing the reaction at 90-110° C. for 3-5 h to obtain a gray-black solid for standby use; S4: grinding the material to ball mill medium in a ratio of 1:3 to a particle size of 500-900 meshes using an ultrafine ball mill, washing with deionized water for 3-5 times, and freeze-drying to obtain the graphene oxide modified ammonium polyphosphate.

3. An organic heat carrier flash point improver according to claim 1, characterized in that: The high flash point solvent oil is an aromatic solvent oil with a flash point greater than 100° C. measured by a closed cup method; the antioxidant is any one of isooctyl propionate, p-phenylenediamine, and dihydroquinoline; and the flocculant is any one of polyacrylate and polymethacrylate.

4. A method for preparing the organic heat carrier flash point improver as claimed in claim 1, characterized in that: The steps include: Step 1: preparing graphene oxide modified ammonium polyphosphate; Step 2: Add the graphene oxide modified ammonium polyphosphate and N,N'-disalicylidenepropylenediamine prepared in step 1 in a certain proportion to high flash point solvent oil in sequence, heat to 60-120°C, and stir for 10-60 min; continue to add a certain proportion of antioxidant and flocculant, stir for 30-90 minutes, and obtain an organic heat carrier flash point improver.

5. A device for preparing the organic heat carrier flash point improver as claimed in claim 1, characterized in that: The ball mill used in step S4 comprises a base (1), the top of the base (1) is rotatably connected to a rotating frame (2), the outer wall of the rotating frame (2) is rotatably connected to a rotating cylinder (3), the outer wall of the rotating cylinder (3) is fixedly connected to a gear ring (4), a first motor (5) is arranged at the top of the base (1), the output end of the first motor (5) is connected to a first spur gear (6), the first spur gear (6) is in contact with the gear ring (4), the first spur gear (6) is meshed with the gear ring (4), the rotating cylinder (3) performs a crushing operation on the material through a crushing mechanism (7), and the rotating cylinder (3) performs a discharging operation through a discharging mechanism (8).

6. The preparation device of an organic heat carrier flash point improver according to claim 5, characterized in that: The crushing mechanism (7) comprises a first transverse plate (701), the first transverse plate (701) being fixedly connected to the inner wall of the rotating cylinder (3) at equal distances around the circumference, a push plate (702) being slidably connected to one end of the inner wall of the rotating cylinder (3), a grid cylinder (703) being fixedly connected to the outer wall of the push plate (702), the inner wall of the grid cylinder (703) being fixedly connected to the second transverse plate (704) at equal distances around the circumference, an annular cover (705) being provided at one end of the rotating cylinder (3), a baffle (709) being provided in the inner cavity of the annular cover (705), a through hole (706) being provided on the outer wall of the annular cover (705), a mounting hole (707) being provided at a position where the outer wall of the rotating cylinder (3) and the through hole (706) are connected, and the inner wall of the mounting hole (707) being threadedly connected to the inner wall of the mounting hole (707). A bolt (708) is provided, the outer wall of the grid tube (703) is symmetrically provided with slots (710) in the upper and lower parts, the inner wall of the annular cover (705) is symmetrically provided with fixing grooves (711) in the upper and lower parts, the outer wall of one end of the baffle plate (709) is rotatably connected to a rotating column (712), one end of the rotating column (712) is fixedly connected to a first bevel gear (713), the inner part of the baffle plate (709) is located on the outer wall of the first bevel gear (713) and is rotatably connected to a second bevel gear (714), the inner wall of the second bevel gear (714) is fixedly connected to a first threaded rod (715), both ends of the first threaded rod (715) are connected to fixing blocks (716), and the fixing blocks (716) are slidably connected to the inner part of the baffle plate (709) and extend out of the baffle plate (709).

7. The preparation device of an organic heat carrier flash point improver according to claim 6, characterized in that: The discharging mechanism (8) comprises a connecting column (801), wherein the connecting column (801) is fixedly connected to one end of the rotating cylinder (3); a displacement rod (802) extending to the bottom end of the connecting column (801) is slidably connected inside the base (1); a second motor (804) is installed at the top end of the base (1) and located on one side of the displacement rod (802); a second threaded rod (803) is connected to the output end of the second motor (804); a second spur gear (805) is rotatably connected to the outer wall of the displacement rod (802) inside the base (1); a displacement seat (806) is slidably connected to the outer wall of the second spur gear (805) inside the base (1); the first motor (5) is installed at the top end of the displacement seat (806); the base The interior of the base (1) is located below the first spur gear (6) and is rotatably connected to a third spur gear (807); one end of the third spur gear (807) is fixedly connected to a rotating disk (808); one end of the base (1) is provided with a groove (809); the inner wall of the groove (809) is fixedly connected to a limiting column (811); the outer wall of the limiting column (811) is slidably connected to a shaking seat (810); the inner cavity of the shaking seat (810) is provided with a collecting seat (812); the top of the collecting seat (812) is provided with a placing seat (813); one end of the rotating disk (808) is fixedly connected to a sliding rod (814); the outer wall of the shaking seat (810) is provided with a sliding groove (815); and the inner wall of the placing seat (813) is fixedly connected to a grid plate (816).

8. The preparation device of an organic heat carrier flash point improver according to claim 6, characterized in that: The inner walls of the slot (710) and the fixing groove (711) are fitted with the outer wall of the fixing block (716); the first bevel gear (713) is meshed with the second bevel gear (714); the outer wall of the first threaded rod (715) is symmetrically provided with external threads; the inner wall of the fixing block (716) is provided with a first threaded hole; the external thread matches the first threaded hole.

9. The preparation device of an organic heat carrier flash point improver according to claim 7, characterized in that: The outer walls of the displacement rod (802) and the displacement seat (806) are both provided with tooth grooves, the tooth grooves meshing with the second spur gear (805), the outer wall of the displacement rod (802) is provided with a second threaded hole, the second threaded hole matches the second threaded rod (803), the first spur gear (6) meshes with the third spur gear (807), the outer wall of the sliding rod (814) fits with the inner wall of the sliding groove (815), the outer wall of the rocking seat (810) is provided with a limiting hole, the inner wall of the limiting hole fits with the outer wall of the limiting column (811).

10. The preparation device of an organic heat carrier flash point improver according to claim 7, characterized in that: A guide column (9) extending into the interior of the displacement seat (806) is fixedly connected to the interior of the base (1); a guide groove (10) is provided at the bottom end of the displacement seat (806); an outer wall of the guide column (9) fits in contact with an inner wall of the guide groove (10); and the outer wall of the guide column (9) is square in shape.

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