CN114632435A - Preparation device and method of high-flash-point solvent and application of preparation device - Google Patents

Preparation device and method of high-flash-point solvent and application of preparation device Download PDF

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CN114632435A
CN114632435A CN202210280821.XA CN202210280821A CN114632435A CN 114632435 A CN114632435 A CN 114632435A CN 202210280821 A CN202210280821 A CN 202210280821A CN 114632435 A CN114632435 A CN 114632435A
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solvent
flash point
push
flash
mixing
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CN114632435B (en
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谢海
唐帆
钱金均
胡明
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Moumou Holding Group Co ltd
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Moumou Holding Group Co ltd
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N25/00Investigating or analyzing materials by the use of thermal means
    • G01N25/50Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility
    • G01N25/52Investigating or analyzing materials by the use of thermal means by investigating flash-point; by investigating explosibility by determining flash-point of liquids

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Abstract

The invention discloses a preparation device and a preparation method of a high-flash-point solvent and application thereof, relating to the technical field of preparation of high-flash-point coatings, and the preparation method comprises the following steps of (A) preparing a plurality of flash-point test samples with different proportions by adopting the preparation device of the high-flash-point solvent; (B) vortex and oscillate samples 1, 2 and 3 … … N one by one, then sequentially put into a closed flash point tester to measure the flash point of the mixed solvent, and a curve is drawn by taking the volume fraction of the solvent I or the solvent II as an abscissa and taking the flash point value as an ordinate; (C) and (4) screening the position with the maximum slope from the curve to serve as the optimal proportion of the mixed solvent, and mixing and preparing the high-flash-point solvent according to the optimal proportion. According to the invention, the preparation of a plurality of proportioning gradient samples can be rapidly and continuously carried out through the preparation device of the high-flash-point solvent, manual repeated weighing and preparation are not required, and the samples are taken out according to the ascending gradient sequence, so that mistakes and omissions are avoided. Meanwhile, the whole preparation process of the high-flash-point solvent is in a totally-enclosed environment, so that the solvent is not easy to volatilize to cause danger, and the safety is good.

Description

Preparation device and method of high-flash-point solvent and application of preparation device
Technical Field
The invention relates to the technical field of high-flash-point coating preparation, in particular to a preparation device and method of a high-flash-point solvent and application of the high-flash-point solvent.
Background
The flash point is the lowest temperature at which a mixture of steam and air formed on the surface of a volatile combustible liquid burns in the presence of a fire, and is one of the important physical parameters for measuring the flammability of compounds, and the lower the flash point, the greater the risk.
A large amount of flammable liquid is used as a solvent in the production of the coating, common solvents comprise toluene, xylene, No. 200 solvent naphtha, n-butyl alcohol, isobutyl alcohol, isopropanol, ethyl acetate, butyl acetate, acetone, methyl ethyl ketone, cyclohexanone, styrene, butyl acrylate, methyl acrylate and the like, and the solvents and additives are generally flammable liquid or flammable liquid and have low flash points. Therefore, the flash point of the coating depends on the flash point of the used solvent, the flash point is low and volatile, and fire or explosion accidents are easily caused in the production, storage, transportation and construction processes of the coating. The flash points of pure components of the solvent used in the coating can be generally obtained through literature data, but with the continuous development of chemical industry and the diversification of chemical products, different solvents are often mixed for use, and the flash point data is difficult to obtain through the literature data.
The existing methods for improving the flash point are mostly to add a non-combustible or flame-retardant solvent into a common solvent, but the flash point value of a mixed solvent can be improved when the volume fraction of the non-combustible or flame-retardant solvent is added, which is usually difficult to determine, a plurality of groups of different mixing ratios need to be set, the flash point values of the mixed solutions with different ratios are measured, a correlation curve of the volume fraction and the flash point is made through the measured values, the optimal mixing ratio is obtained through the curve, and the change rule of the flash point of the mixed solvent along with the ratio is rapidly determined through the curve.
At present, because the volatile combustible explosive nature of solvent, the ratio between the different solvents is the manual work of adopting and is gone on in the fume hood more, because the gradient of ratio sets up more, the preparation of mixed solvent sample is wasted time and energy, when fumbling the best ratio of a plurality of different solvent combinations, and work load promotes by a wide margin, appears the phenomenon such as mismatching, hourglass join in marriage very easily.
Disclosure of Invention
The invention aims to provide a preparation device and a preparation method of a high-flash-point solvent and application of the preparation device and the preparation method, and aims to solve the problem that the conventional high-flash-point solvent is inconvenient to match.
In order to solve the above problems, the present invention provides the following technical solutions:
a preparation device of a high flash point solvent comprises a rack, wherein one side of the rack is provided with a layer-by-layer ejection cup assembly, the inner side of the layer-by-layer ejection cup assembly is communicated with a plurality of liquid inlet pipes at equal intervals from top to bottom, a liquid injection cylinder is inserted in each liquid inlet pipe, a push injection rod is connected in the liquid injection cylinder in a sealing and sliding manner, the other side of the rack is provided with a transverse translation mechanism, each transverse translation mechanism is provided with a stand column and a guide column, each stand column is arranged between the layer-by-layer ejection cup assembly and the guide column, each stand column is provided with a plurality of horizontal push assemblies, the lengths of the horizontal push assemblies are gradually increased from bottom to top, the horizontal push assemblies and the push injection rods are in one-to-one correspondence and coaxial arrangement, the inner sides of the guide columns are connected with a step push plate in a sliding manner, the outer ends of the horizontal push assemblies are in rolling butt joint with the inner sides of the step push plate, and the bottoms of the step push plate are in sliding connection with the transverse translation mechanism, a second ejector rod is arranged below the stepped push plate, a lifting mechanism is arranged at the lower part of the rack, the lower end of the second ejector rod is movably connected to the lifting mechanism, the lower end of the layer-by-layer ejection cup assembly is fixedly arranged on the lifting mechanism, the stepped push plate synchronously and periodically extrudes the horizontal push assembly in the ascending process, and a solvent in the liquid injection cylinder is injected into the layer-by-layer ejection cup assembly in the ascending process in multiple times through the horizontal push assembly.
Preferably, the layer-by-layer cup jacking assembly comprises a vertical pipe arranged on the rack, a plurality of dry mixing cups are slidably connected in the vertical pipe, the mixing cups are stacked one by one in the vertical pipe, the top of each mixing cup is periodically communicated with the liquid inlet pipe in the process of being jacked up, a top plate is abutted to the lower part of each mixing cup at the bottom, the top plate is slidably connected with the inner wall of the vertical pipe, a first jacking rod is arranged below the top plate, and the lower end of the first jacking rod is fixedly arranged on the lifting mechanism.
Preferably, the outer wall of the mixing cup is provided with a limiting slide block, the inner wall of the vertical pipe is provided with a sliding groove, the limiting slide block is connected in the sliding groove in a sliding manner, the top of the mixing cup is provided with a U-shaped notch, and the notch is positioned below the nearest liquid inlet pipe.
Preferably, the flat push subassembly is including transversely locating the well cavity section of thick bamboo on the stand, and the axial sliding connection of well cavity section of thick bamboo has the push rod, sliding connection has the separation blade in the well cavity section of thick bamboo, the separation blade sets firmly on the push rod, be equipped with the spring between separation blade and the interior end of well cavity section of thick bamboo, outside the push rod was located to the spring housing, the interior end of push rod is worn out well cavity section of thick bamboo and is equipped with the fixture block, fixture block and push rod all with inject the coaxial setting of pole, the outer end of push rod is also worn out well cavity section of thick bamboo and is equipped with the pulley, pulley roll butt in the inboard of ladder push pedal, the length of a plurality of push rods increases gradually from bottom to top, and the inner of a plurality of push rods all aligns the setting.
Preferably, the step push plate is narrow at the top and wide at the bottom, an inclined plane and a vertical plane appear on the inner side of the step push plate repeatedly and alternately, sliding rails are arranged on the inclined plane and the vertical plane, and the pulleys are arranged in the sliding rails.
Preferably, horizontal translation mechanism includes translation slider, the frame top is equipped with logical groove, translation slider sliding connection leads to the inslot, translation slider's inboard and outside are located respectively to stand and guide post, be equipped with the lift mouth on the translation slider, the bottom sliding connection of ladder push pedal is in the lift mouth, the lift mouth is located to the upper end of ejector pin two, it is connected with screw rod one to lead to the inslot transverse rotation, translation slider and a screw rod threaded connection.
Preferably, elevating system includes the lifter plate with frame both sides sliding connection, vertical rotation is connected with screw rod two in the frame, the lifter plate is connected with screw rod two threaded connection, the lower extreme and the lifter plate of ejector pin one link firmly, be equipped with the translation groove on the lifter plate, the lower extreme sliding connection of ejector pin two is in the translation inslot, the side intercommunication in translation groove has the fixed slot, be equipped with stop screw in the fixed slot.
A preparation method of a high flash point solvent comprises the following specific steps:
(A) a plurality of flash point test samples with different proportions are prepared by adopting the preparation device of the high flash point solvent, and the method comprises the following steps: sucking an equal amount of a first solvent into each liquid injection cylinder, inserting a front port of each liquid injection cylinder into a liquid inlet pipe, fixing the liquid injection cylinders, adding an equal amount of a second solvent into each mixing cup, stacking the solvents in a vertical pipe, rotating the first screw until an injection rod is clamped in the clamping block and abutted against the clamping block, rotating the second screw, simultaneously lifting the stepped push plate and the mixing cup, stopping rotating the second screw after the mixing cup on the uppermost layer is ejected out of most parts of the vertical pipe, taking out the mixing cup and sealing the mixing cup to serve as the first sample, continuing rotating the second screw until the next mixing cup is ejected out of most parts, taking out the mixing cup and sealing the mixing cup to serve as the second sample, repeating the operation until the mixing cup on the bottommost part is ejected out to serve as the first sample N, and increasing the volume fraction of the first solvent in the samples 1-N one by one, so as to finish the preparation of a series of samples with different proportions one by one;
(B) vortex and oscillate samples 1, 2 and 3 … … N one by one, then sequentially put into a closed flash point tester to measure the flash point of the mixed solvent, and a curve is drawn by taking the volume fraction of the solvent I or the solvent II as an abscissa and taking the flash point value as an ordinate;
(C) and (4) screening the position with the maximum slope from the curve to serve as the optimal proportion of the mixed solvent, and mixing and preparing the high-flash-point solvent according to the optimal proportion to obtain the high-flash-point solvent.
Preferably, the high-flash-point solvent is prepared by mixing No. 200 solvent oil and triethyl phosphate according to a volume ratio of 4: 7.
The application of the high flash point solvent is to use the high flash point solvent in preparing a high flash point coating.
The invention has the advantages that:
according to the invention, the preparation device of the high-flash-point solvent can be used for rapidly and continuously preparing a plurality of proportioning gradient samples without manual repeated weighing and preparation, and the mixing cups are ejected one by one according to the ascending gradient sequence during sample outlet, so that no error or leakage occurs. Meanwhile, the whole preparation process of the high-flash-point solvent is in a totally-enclosed environment, so that the solvent is not easy to volatilize to cause danger, and the safety is good. The preparation device utilizing the high-flash-point solvent can greatly shorten the weighing and preparing time of the solvent and reduce the labor intensity, well avoid fatigue and low efficiency caused by manual large-batch weighing operation, reduce the interference of human factors on flash point value measurement, and have more gradient settings and more obvious advantages in various aspects of the preparation device of the high-flash-point solvent. The preparation device of the high-flash-point solvent is simple to operate, the amount of single injection can be adjusted at will, the preset proportion is automatically completed, the mixing proportion is not required to be recorded after preparation, the operation amount is greatly reduced, and the exploration efficiency of the high-flash-point solvent formula is improved.
The preparation device for the high flash point solvent can add the liquid solvent into the mixing cups which move upwards step by pushing the stepped push plate upwards, can rapidly complete multiple periodical and synchronous solvent addition into a plurality of mixing cups by matching with the push rods with gradually increasing lengths, increases the addition times along with the increase of the lengths of the push rods, is extremely simple and convenient in operation process, and is suitable for large-batch and multi-group solvent mixing.
Drawings
Fig. 1 and 2 are schematic diagrams of the overall structure of a high flash point solvent preparation device under different viewing angles.
FIG. 3 is a top view of a high flash point solvent manufacturing apparatus.
Fig. 4 is a sectional view taken along line a-a in fig. 3.
Fig. 5 is a schematic structural view of the mixing cup.
FIG. 6 is a graph showing the correlation between the flash point value and the solvent ratio in example 1.
FIG. 7 is a graph showing the correlation between the flash point value and the solvent ratio in examples 2 to 6.
The device comprises a rack 1, a through groove 11, a vertical pipe 2, a top rod I21, a liquid injection cylinder 22, a liquid injection rod 221, a liquid inlet pipe 23, a top plate 24, a sliding groove 25, a mixing cup 3, a notch 31, a limiting slide block 32, a vertical column 4, a hollow cylinder 41, a push rod 5, a pulley 51, a fixture block 52, a baffle 53, a spring 54, a stepped push plate 6, a top rod II 61, a sliding rail 62, a vertical plane 63, a slope 64, a guide column 7, a translation slide block 8, a screw rod I81, a lifting port 82, a lifting plate 9, a screw rod II 91, a translation groove 92, a fixing groove 93 and a limiting screw 94.
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
Example 1: the preparation of the mixed high flash point solvent of cyclohexanone and carbon tetrachloride was carried out using the high flash point solvent preparation apparatus shown in FIGS. 1 to 4.
The preparation device of the high-flash-point solvent comprises a frame 1, wherein one side of the frame 1 is provided with a layer-by-layer top cup assembly, the inner side of the layer-by-layer top cup assembly is communicated with a plurality of liquid inlet pipes 23 at equal intervals from top to bottom, liquid injection cylinders 22 are inserted in the liquid inlet pipes 23, the liquid injection cylinders 22 are connected with an injection rod 221 in a sealing and sliding manner, the other side of the frame 1 is provided with a transverse translation mechanism, the transverse translation mechanism is provided with stand columns 4 and guide columns 7, the stand columns 4 are arranged between the layer-by-layer top cup assembly and the guide columns 7, the stand columns 4 are provided with a plurality of flat push assemblies, the lengths of the flat push assemblies are gradually increased from bottom to top, the flat push assemblies and the injection rods 221 are in one-to-one correspondence and coaxial arrangement, the inner sides of the guide columns 7 are connected with a step push plate 6 in a sliding manner, the outer ends of the flat push assemblies are all in rolling and abutting contact with the inner sides of the step push plate 6, the bottoms of the step push plate 6 are in a sliding manner, a second ejector rod 61 is arranged below the stepped push plate 6, a lifting mechanism is arranged at the lower part of the rack 1, the lower end of the second ejector rod 61 is movably connected to the lifting mechanism, the lower end of the layer-by-layer top cup component is fixedly arranged on the lifting mechanism, the stepped push plate 6 synchronously and periodically extrudes the horizontal push component in an ascending process, and the solvent in the liquid injection cylinder 22 is injected into the layer-by-layer top cup component in the ascending process in times through the horizontal push component. The layer-by-layer cup jacking assembly comprises a vertical pipe 2 arranged on a rack 1, a plurality of dry mixing cups 3 are slidably connected in the vertical pipe 2, the mixing cups 3 are stacked one by one in the vertical pipe 2, the top parts of the mixing cups 3 are periodically communicated with a liquid inlet pipe 23 in the process of being jacked up, a top plate 24 is abutted to the lower part of the mixing cup 3 at the bottom, the top plate 24 is slidably connected with the inner wall of the vertical pipe 2, a first jacking rod 21 is arranged below the top plate 24, and the lower end of the first jacking rod 21 is fixedly arranged on a lifting mechanism. In this embodiment, the number of the horizontal pushing components, the liquid inlet pipe 23, the liquid injection cylinder 22 and the mixing cup 3 is 10, and if necessary, more proportioning gradients are set, and the number of the components can be increased as required.
As shown in fig. 5, the outer wall of the mixing cup 3 is provided with a limiting slide block 32, the inner wall of the vertical pipe 2 is provided with a sliding groove 25, the limiting slide block 32 is slidably connected in the sliding groove 25, the top of the mixing cup 3 is provided with a U-shaped notch 31, and the notch 31 is located below the nearest liquid inlet pipe 23. The limiting slide block 32 can prevent the mixing cup 3 from rotating in the stand pipe 2, so that the gap 31 cannot be communicated with the liquid inlet pipe 23.
The flat push subassembly is including transversely locating a cavity section of thick bamboo 41 on stand 4, and the axial sliding connection of a cavity section of thick bamboo 41 has push rod 5, sliding connection has separation blade 53 in a cavity section of thick bamboo 41, separation blade 53 sets firmly on push rod 5, be equipped with spring 54 between separation blade 53 and the interior of a cavity section of thick bamboo 41, outside push rod 5 was located to spring 54 cover, a cavity section of thick bamboo 41 and be equipped with fixture block 52 are worn out to the inner of push rod 5, fixture block 52 and push rod 5 all with inject the coaxial setting of pole 221, a cavity section of thick bamboo 41 and be equipped with pulley 51 are also worn out to the outer end of push rod 5, pulley 51 rolls the butt in the inboard of ladder push pedal 6, and the length of a plurality of push rods 5 increases progressively from bottom to top, and the inner of a plurality of push rods 5 all aligns the setting. The stepped push plate 6 is narrow at the top and wide at the bottom, the inner side of the stepped push plate 6 repeatedly and alternately forms an inclined surface 64 and a vertical surface 63, the inclined surface 64 and the vertical surface 63 are both provided with a sliding rail 62, and the pulley 51 is arranged in the sliding rail 62.
Horizontal translation mechanism includes translation slider 8, 1 top in the frame is equipped with logical groove 11, 8 sliding connection of translation slider are in leading to groove 11, the inboard and the outside of translation slider 8 are located respectively to stand 4 and guide post 7, be equipped with lift mouth 82 on the translation slider 8, the bottom sliding connection of ladder push pedal 6 is in lift mouth 82, in lift mouth 82 is located to the upper end of two 61 ejector pins, it is connected with screw rod 81 to lead to the inslot transverse rotation of 11, translation slider 8 and screw rod 81 threaded connection.
Elevating system includes the lifter plate 9 with 1 both sides sliding connection of frame, vertical rotation is connected with two 91 of screw rods in the frame 1, lifter plate 9 and two 91 threaded connection of screw rods, the lower extreme of ejector pin 21 links firmly with lifter plate 9, be equipped with translation groove 92 on the lifter plate 9, the lower extreme sliding connection of two 61 of ejector pins is in translation groove 92, the side intercommunication in translation groove 92 has fixed slot 93, be equipped with stop screw 94 in the fixed slot 93.
The specific preparation method of the high flash point mixed solvent comprises the following steps:
(A) the preparation device of the high-flash-point solvent is adopted to prepare a plurality of flash-point test samples with different proportions, and the method comprises the following steps: adding 10mL of cyclohexanone in equal amount into each mixing cup 3, stacking the cyclohexanone in the vertical pipe 2 in an overlapped mode, sucking 30mL of carbon tetrachloride into each liquid injection cylinder 22, inserting the front end of each liquid injection cylinder 22 into the liquid inlet pipe 23 one by one, fixing the liquid injection cylinders 22, flushing the bottom of each mixing cup 3 with the liquid inlet pipe 23 and blocking the liquid inlet pipe 23 when in an initial position, wherein the notch 31 is located below the liquid inlet pipe 23 but not communicated, and in addition, the pulley 51 is located at an internal corner formed by the vertical surface 63 and the inclined surface 64. Rotating the first screw 81, the translational slide block 8 drives the upright column 4, the horizontal pushing assembly, the stepped push plate 6 and the guide column 7 to approach the pushing rod 221 in the same direction until the pushing rod 221 is clamped in the clamping block 52 and abutted against the clamping block, locking the limit screw 94, fixing the lower end of the second ejector rod 61 on the lifting plate 9, rotating the second screw 91, synchronously driving the second ejector rod 61 and the first ejector rod 21 to move upwards by the lifting plate 9, lifting the stepped push plate 6 by the second ejector rod 61, pushing the mixing cup 3 by the first ejector rod 21 through the top plate 24, in the ascending process of the stepped push plate 6, the pulley 51 rolls downwards on the inclined plane 64, the push rod 5 is synchronously pushed inwards for a certain distance, the length of the distance can be controlled by the angle of the inclined plane 64, the push rod 5 drives the clamping block 52 to push the pushing rod 221 to move transversely, when the pushing rod 221 moves transversely, the solvent in the liquid injection cylinder 22 is injected into the liquid inlet pipe 23 through the front end opening, while pushing the pushing rod 221, the mixing cups 3 move upwards synchronously, just the liquid inlet pipe 23 is communicated with the gap 31, carbon tetrachloride is injected into the mixing cups 3, the pulley 51 enters the vertical surface 63 along with the continuous ascending of the mixing cups 3 and the stepped push plate 6, the push rod 5 does not move transversely and keeps the current position, the push rod 5 enables the pulley 51 to be always abutted against the inclined surface 64 or the vertical surface 63 under the action of the spring 54 and the baffle plate 53, the solvent adding process is completed at the moment, the gap 31 of the mixing cups 3 also moves above the liquid inlet pipe 23, the liquid inlet pipe 23 is closed again, the screw rod two 91 continues to rotate until the mixing cup 3 at the uppermost layer is ejected from most parts of the vertical pipe 2, the screw rod two 91 stops rotating, the mixing cup 3 is taken out and sealed to be used as a sample one, the screw rod two 91 continues to rotate until the next mixing cup 3 is ejected from most parts, the mixing cup 3 is taken out and sealed to be used as a sample two, repeating the operation until the mixing cup 3 at the bottommost part is ejected out as a sample N, taking out one mixing cup 3 every time the mixing cup is ejected out, and synchronously adding carbon tetrachloride once in the remaining mixing cups 3 in the stand pipe 2, so that the volume fractions of the carbon tetrachloride in the samples 1-N are gradually increased one by one, and thus, the preparation of a series of samples with different ratios is completed. After all the mixing cups 3 are taken out, the screw rod I81 is rotated reversely, so that the fixture block 52 is separated from the injection rod 221, all the liquid injection cylinders 22 are taken down, the screw rod II 91 is rotated reversely, the ejector rod I21 and the ejector rod II 61 are moved downwards, the mixing cups 3 are loaded into the vertical pipe 2 one by one in the downward moving process, the push rod 5 is completely reset under the action of the spring 54 in the downward moving process of the stepped push plate 6, and the operations are repeated to continue to mix the other solvents in proportion.
(B) The flash point determination test is carried out according to GB/T21615-2008 'dangerous goods-flammable liquid closed cup flash point test method'. Before the test, a sample testing cup of the flash point instrument is cleaned by absolute ethyl alcohol and dried in the air, so that the influence of the ethyl alcohol on the test result is prevented; setting the tester to the test temperature, after the temperature is stable, respectively pouring a proper amount of liquid into the test cup after the samples 1, 2 and 3 … … N are vortex-oscillated one by one, and covering the test cup cover. The ignition test is repeated, when a blue flame appears above the liquid level of the sample initially, the reading of the thermometer is used as the measurement result of the flash point, if the flash fire occurs, the temperature of the measuring device is reduced until the flash fire does not occur, if the flash fire does not occur, the sample is replaced to carry out the test again, and the measurement result is not effective until the test can be repeated. And drawing a curve by taking the volume ratio of cyclohexanone to carbon tetrachloride as an abscissa and the measured flash point value as an ordinate.
(C) And (4) screening the position with the maximum slope from the curve to serve as the optimal proportion of the mixed solvent, and mixing and preparing the high-flash-point solvent according to the optimal proportion to obtain the high-flash-point solvent.
TABLE 1 Cyclohexanone to carbon tetrachloride ratio Table
Sample numbering Cyclohexanone volume (mL) Volume of carbon tetrachloride (mL) Volume ratio of
0 10 0 -
1 10 2.5 4:1
2 10 5 4:2
3 10 7.5 4:3
4 10 10 4:4
5 10 12.5 4:5
6 10 15 4:6
7 10 17.5 4:7
8 10 20 4:8
9 10 22.5 4:9
10 10 25 4:10
As can be seen from FIG. 6, when the ratio of cyclohexanone to carbon tetrachloride is between 4:5 and 4:6, the flash point value is greatly increased, and the increase of the flash point value by continuously increasing the amount of carbon tetrachloride is limited, so that the ratio of 4:6 can be selected as the preparation ratio of the high-flash-point mixed solvent.
Example 2: the remainder was the same as in example 1 except that cyclohexanone was replaced with toluene and carbon tetrachloride with isobutanol. As shown in fig. 7, the flash point value of the mixed solvent of isobutanol and toluene is mostly below 10 ℃, which is probably because toluene dilutes hydrogen bonds in isobutanol and weakens intermolecular forces, so that isobutanol is difficult to pull up the flash point value of the mixed solvent.
Example 3: the remainder was the same as in example 1 except that cyclohexanone was replaced with No. 200 mineral spirits and carbon tetrachloride was replaced with triethyl phosphate. As shown in FIG. 7, the ratio of 4:7 can be selected as the preparation ratio of the high flash point mixed solvent because the flash point value of the mixed solvent is greatly increased between 4:6 and 4: 7.
Example 4: the remainder was the same as in example 1 except that cyclohexanone was replaced with D40 mineral spirit and carbon tetrachloride was replaced with triethyl phosphate. As shown in FIG. 7, the same principle can be used to select the same volume ratio as the preparation ratio of the high flash point mixed solvent.
Example 5: the rest of the process was the same as in example 1 except that cyclohexanone was replaced with n-butanol and carbon tetrachloride was replaced with butyl acetate. As shown in fig. 7, the flash point values of the mixed solvents were not in a proportion of a large jump, and the flash point values were all low, and were not used as an alternative high flash point solvent combination. The principle of flash point change was the same as in example 2.
Example 6: the procedure of example 1 was repeated except that cyclohexanone was replaced with xylene and carbon tetrachloride was replaced with propylene glycol methyl ether acetate. As shown in fig. 7, the flash point value of the mixed solvent changes more gradually, and the overall flash point values are all lower, and the mixed solvent is not used as a high-flash-point solvent.
The operation of the embodiments 1 to 6 is continuously completed, the average configuration time of the single sample in the embodiments 1 to 6 is counted, after the operation is performed by adopting the mixed solvent proportioning device, the average sample outlet time of the single sample in the embodiments 1 to 6 only needs 10s, and the average time of the manual preparation reaches more than 1 min.
Example 7: the high flash point solvent prepared by mixing mineral spirit No. 200 of example 3 with triethyl phosphate in a 4:7 volume ratio was used to prepare the high flash point coating: adding 4-13 parts by weight of epoxy resin polymer, 0.5-1 part by weight of ammonium polyphosphate, 0.5-1 part by weight of binder, 5-17 parts by weight of epoxy resin, 1-1.5 parts by weight of corrosion inhibitor, 3-7 parts by weight of defoaming agent, 2-10 parts by weight of ultraviolet absorbent, 3-6 parts by weight of titanium dioxide and 3-7 parts by weight of high flash point solvent into a mixing and stirring device, fully stirring, adding into a homogenizer, and homogenizing to obtain the high flash point coating, wherein the flash point value of the high flash point coating is 82 ℃.
It will be appreciated by those skilled in the art that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The embodiments disclosed above are therefore to be considered in all respects as illustrative and not restrictive. All changes which come within the scope of or are equivalent to the scope of the invention are intended to be embraced therein.

Claims (10)

1. The preparation device of the high flash point solvent is characterized by comprising a rack (1), wherein one side of the rack (1) is provided with a layer-by-layer ejection cup assembly, the inner side of the layer-by-layer ejection cup assembly is communicated with a plurality of liquid inlet pipes (23) at equal intervals from top to bottom, liquid injection cylinders (22) are inserted in the liquid inlet pipes (23), the liquid injection cylinders (22) are internally sealed and slidably connected with ejection rods (221), the other side of the rack (1) is provided with a transverse translation mechanism, the transverse translation mechanism is provided with stand columns (4) and guide columns (7), the stand columns (4) are arranged between the layer-by-layer ejection cup assembly and the guide columns (7), the stand columns (4) are provided with a plurality of flat push assemblies, the lengths of the flat push assemblies are gradually increased from bottom to top, the flat push assemblies and the ejection rods (221) are in one-to-one correspondence and coaxial arrangement, the inner sides of the guide columns (7) are slidably connected with stepped push plates (6), the outer end of flat push subassembly all rolls the butt with the inboard of ladder push pedal (6), the bottom and the horizontal translation mechanism sliding connection of ladder push pedal (6), ladder push pedal (6) have ejector pin two (61), the lower part of frame (1) is equipped with elevating system, ejector pin two (61) lower extreme swing joint is on elevating system, the lower extreme of successive layer top cup subassembly sets firmly on elevating system, ladder push pedal (6) are at the ascending in-process synchronous periodically extrudees the flat push subassembly, through the flat push subassembly with annotate the solvent fractional injection in liquid section of thick bamboo (22) go upward in the successive layer top cup subassembly.
2. The device for preparing the high flash point solvent according to claim 1, wherein the layer-by-layer top cup assembly comprises a vertical pipe (2) arranged on the frame (1), a plurality of mixing cups (3) are slidably connected in the vertical pipe (2), the mixing cups (3) are stacked one by one in the vertical pipe (2), the mixing cups (3) are lifted up, the top of the mixing cups (3) are periodically communicated with the liquid inlet pipe (23), the bottom mixing cup (3) is abutted with the top plate (24), the top plate (24) is slidably connected with the inner wall of the vertical pipe (2), a first ejector rod (21) is arranged below the top plate (24), and the lower end of the first ejector rod (21) is fixedly arranged on the lifting mechanism.
3. The device for preparing the high flash point solvent according to claim 2, wherein the outer wall of the mixing cup (3) is provided with a limiting slide block (32), the inner wall of the vertical pipe (2) is provided with a sliding groove (25), the limiting slide block (32) is slidably connected in the sliding groove (25), the top of the mixing cup (3) is provided with a U-shaped notch (31), and the notch (31) is located below the nearest liquid inlet pipe (23).
4. The device for preparing the high flash point solvent according to claim 1, wherein the horizontal pushing assembly comprises a hollow cylinder (41) transversely arranged on the upright post (4), the axial sliding of the hollow cylinder (41) is connected with a push rod (5), the sliding of the hollow cylinder (41) is connected with a baffle (53), the baffle (53) is fixedly arranged on the push rod (5), a spring (54) is arranged between the baffle (53) and the inner end of the hollow cylinder (41), the spring (54) is sleeved outside the push rod (5), the inner end of the push rod (5) penetrates through the hollow cylinder (41) and is provided with a clamping block (52), the clamping block (52) and the push rod (5) are coaxially arranged with the injection rod (221), the outer end of the push rod (5) also penetrates through the hollow cylinder (41) and is provided with a pulley (51), the pulley (51) is in rolling contact with the inner side of the stepped push plate (6), the lengths of the push rods (5) are gradually increased from bottom to top, and the inner ends of the push rods (5) are arranged in an aligned mode.
5. The device for preparing the high flash point solvent according to claim 4, wherein the step push plate (6) is narrow at the top and wide at the bottom, the inner side of the step push plate (6) repeatedly and alternately presents a slope (64) and a vertical surface (63), the slope (64) and the vertical surface (63) are both provided with a slide rail (62), and the pulley (51) is arranged in the slide rail (62).
6. The device for preparing the high flash point solvent according to claim 1, wherein the transverse translation mechanism comprises a translation sliding block (8), a through groove (11) is formed in the top of the frame (1), the translation sliding block (8) is slidably connected in the through groove (11), the upright post (4) and the guide post (7) are respectively arranged on the inner side and the outer side of the translation sliding block (8), a lifting port (82) is formed in the translation sliding block (8), the bottom of the stepped push plate (6) is slidably connected in the lifting port (82), the upper end of the second ejector rod (61) is arranged in the lifting port (82), a first screw rod (81) is transversely rotatably connected in the through groove (11), and the translation sliding block (8) is in threaded connection with the first screw rod (81).
7. The device for preparing the high flash point solvent according to claim 2, wherein the lifting mechanism comprises a lifting plate (9) slidably connected with two sides of the frame (1), a second screw (91) is vertically and rotatably connected to the frame (1), the lifting plate (9) is in threaded connection with the second screw (91), the lower end of the first ejector rod (21) is fixedly connected with the lifting plate (9), a translation groove (92) is formed in the lifting plate (9), the lower end of the second ejector rod (61) is slidably connected in the translation groove (92), a fixing groove (93) is communicated with the side surface of the translation groove (92), and a limit screw (94) is arranged in the fixing groove (93).
8. The preparation method of the high flash point solvent is characterized by comprising the following specific steps:
(A) preparing a plurality of flash point test samples with different proportions by adopting the preparation device of the high flash point solvent as defined in any one of claims 1 to 7, wherein the method comprises the following steps: sucking an equal amount of a first solvent into each liquid injection cylinder, inserting a front port of each liquid injection cylinder into a liquid inlet pipe, fixing the liquid injection cylinders, adding an equal amount of a second solvent into each mixing cup, stacking the solvents in a vertical pipe, rotating the first screw until an injection rod is clamped in the clamping block and abutted against the clamping block, rotating the second screw, simultaneously lifting the stepped push plate and the mixing cup, stopping rotating the second screw after the mixing cup on the uppermost layer is ejected out of most parts of the vertical pipe, taking out the mixing cup and sealing the mixing cup to serve as the first sample, continuing rotating the second screw until the next mixing cup is ejected out of most parts, taking out the mixing cup and sealing the mixing cup to serve as the second sample, repeating the operation until the mixing cup on the bottommost part is ejected out to serve as the first sample N, and increasing the volume fraction of the first solvent in the samples 1-N one by one, so as to finish the preparation of a series of samples with different proportions one by one;
(B) vortex and oscillate samples 1, 2 and 3 … … N one by one, then sequentially put into a closed flash point tester to measure the flash point of the mixed solvent, and a curve is drawn by taking the volume fraction of the solvent I or the solvent II as an abscissa and taking the flash point value as an ordinate;
(C) and (4) screening the position with the maximum slope from the curve to serve as the optimal proportion of the mixed solvent, and mixing and preparing the high-flash-point solvent according to the optimal proportion to obtain the high-flash-point solvent.
9. The method as claimed in claim 8, wherein the high flash point solvent is prepared by mixing No. 200 mineral spirit and triethyl phosphate at a volume ratio of 4: 7.
10. Use of a high flash point solvent according to claim 9 for the preparation of a high flash point coating.
CN202210280821.XA 2022-03-21 2022-03-21 Preparation device and method of high-flash-point solvent and application of preparation device Active CN114632435B (en)

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