CN117505005B - Production system for sodium ethoxide - Google Patents
Production system for sodium ethoxide Download PDFInfo
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- CN117505005B CN117505005B CN202410019000.XA CN202410019000A CN117505005B CN 117505005 B CN117505005 B CN 117505005B CN 202410019000 A CN202410019000 A CN 202410019000A CN 117505005 B CN117505005 B CN 117505005B
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- QDRKDTQENPPHOJ-UHFFFAOYSA-N sodium ethoxide Chemical compound [Na+].CC[O-] QDRKDTQENPPHOJ-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 79
- 238000001514 detection method Methods 0.000 claims abstract description 78
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 73
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000000498 ball milling Methods 0.000 claims abstract description 35
- 238000005070 sampling Methods 0.000 claims abstract description 22
- 230000000712 assembly Effects 0.000 claims abstract description 12
- 238000000429 assembly Methods 0.000 claims abstract description 12
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 5
- 239000010959 steel Substances 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 46
- 239000007788 liquid Substances 0.000 claims description 38
- 238000004891 communication Methods 0.000 claims description 18
- 239000003153 chemical reaction reagent Substances 0.000 claims description 5
- 238000012544 monitoring process Methods 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 3
- 238000005096 rolling process Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 18
- 230000008569 process Effects 0.000 abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 13
- 239000000376 reactant Substances 0.000 description 9
- 229910000365 copper sulfate Inorganic materials 0.000 description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 7
- 230000009471 action Effects 0.000 description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 5
- 239000000292 calcium oxide Substances 0.000 description 5
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 3
- 239000005750 Copper hydroxide Substances 0.000 description 3
- 229910001956 copper hydroxide Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 230000000670 limiting effect Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- YKFCISHFRZHKHY-NGQGLHOPSA-N (2s)-2-amino-3-(3,4-dihydroxyphenyl)-2-methylpropanoic acid;trihydrate Chemical compound O.O.O.OC(=O)[C@](N)(C)CC1=CC=C(O)C(O)=C1.OC(=O)[C@](N)(C)CC1=CC=C(O)C(O)=C1 YKFCISHFRZHKHY-NGQGLHOPSA-N 0.000 description 1
- 241000530268 Lycaena heteronea Species 0.000 description 1
- CXOFVDLJLONNDW-UHFFFAOYSA-N Phenytoin Chemical compound N1C(=O)NC(=O)C1(C=1C=CC=CC=1)C1=CC=CC=C1 CXOFVDLJLONNDW-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- PPWHTZKZQNXVAE-UHFFFAOYSA-N Tetracaine hydrochloride Chemical compound Cl.CCCCNC1=CC=C(C(=O)OCCN(C)C)C=C1 PPWHTZKZQNXVAE-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- -1 ball-milling jar 1 Chemical compound 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229940083181 centrally acting adntiadrenergic agent methyldopa Drugs 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000001037 epileptic effect Effects 0.000 description 1
- JUKPWJGBANNWMW-VWBFHTRKSA-N eplerenone Chemical compound C([C@@H]1[C@]2(C)C[C@H]3O[C@]33[C@@]4(C)CCC(=O)C=C4C[C@H]([C@@H]13)C(=O)OC)C[C@@]21CCC(=O)O1 JUKPWJGBANNWMW-VWBFHTRKSA-N 0.000 description 1
- 229960001208 eplerenone Drugs 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229960002895 phenylbutazone Drugs 0.000 description 1
- VYMDGNCVAMGZFE-UHFFFAOYSA-N phenylbutazonum Chemical compound O=C1C(CCCC)C(=O)N(C=2C=CC=CC=2)N1C1=CC=CC=C1 VYMDGNCVAMGZFE-UHFFFAOYSA-N 0.000 description 1
- 229960002036 phenytoin Drugs 0.000 description 1
- 229950009297 pivoxil Drugs 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000007363 regulatory process Effects 0.000 description 1
- 159000000000 sodium salts Chemical group 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 229960002494 tetracaine hydrochloride Drugs 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Abstract
The invention relates to the technical field of sodium ethoxide production equipment, in particular to a production system for sodium ethoxide, which comprises a ball milling tank, steel balls, a tank cover, a stirring pipe, a fixing ring, a detection component and a sampling component, wherein the tank cover can be fixed at the opening of the top of the ball milling tank; the sampling assembly is used for intermittently sampling from the ball milling tank, and sequentially injecting samples collected before and after into different detection assemblies for detection. According to the invention, the sampling assembly is used for intermittently sampling from the ball milling tank, and the sample is injected into the detection assembly to detect the content of sodium hydroxide, so that whether the sodium hydroxide and the detection assembly react completely can be accurately known, and the time for carrying out the water removal process can be accurately controlled.
Description
Technical Field
The invention relates to the technical field of sodium ethoxide production equipment, in particular to a production system for sodium ethoxide.
Background
The sodium ethoxide is mainly used in medicine and pesticide industry, and the medical products applying the sodium ethoxide are phenytoin, phenylbutazone, epileptic ketone, methyldopa, tetracaine hydrochloride, eplerenone, pivoxil and the like.
At present, in the production and preparation process of sodium ethoxide, for example, chinese patent publication No. CN106045813B, a method for preparing sodium ethoxide by a ball milling method is disclosed, the device is characterized in that prepared absolute ethyl alcohol and sodium hydroxide are placed in a stirring ball mill, the stirring ball mill is operated, after the absolute ethyl alcohol and the sodium hydroxide fully react, a product is led out of the stirring ball mill through a circulating pump, water generated in the ball milling process is removed, then the dehydrated product is filtered through a filtering device, and finally the preparation of sodium ethoxide is completed.
However, when the ball mill is used for stirring to react the anhydrous ethanol and the sodium hydroxide, whether the anhydrous ethanol and the sodium hydroxide are completely reacted or not cannot be accurately known, so that the time from the completion of the reaction to the water removal stage is difficult to control, sodium ethoxide is unstable, sodium ethoxide generated by the reaction is decomposed into ethanol and sodium hydroxide again with water, and other chemical reactions possibly caused by sodium hydroxide contained in the sodium ethoxide solution in the subsequent water removal process can be caused, so that the purity and activity of the sodium ethoxide solution are affected.
Disclosure of Invention
The invention aims to provide a production system for sodium ethoxide, which aims to solve the technical problems.
In order to achieve the above purpose, the present invention provides the following technical solutions: a production system for sodium ethoxide, including ball-milling jar, steel ball and can fix the cover in ball-milling jar top opening part, still include:
the stirring pipe is arranged at the bottom of the tank cover and can rotate, and a plurality of stirring rods are fixed at the lower half section of the stirring pipe;
the stirring pipe penetrates through the inner ring of the fixed ring, an extension pipe is coaxially fixed at the bottom of the fixed ring, a plurality of annularly distributed detection assemblies are mounted on the outer wall of the extension pipe, and the detection assemblies are used for detecting the content of sodium hydroxide;
and the sampling assembly is used for intermittently sampling from the ball milling tank and sequentially injecting the samples collected before and after into different detection assemblies for detection.
Preferably, the sampling assembly comprises a sleeve disc eccentrically fixed at the bottom of the tank cover, a water removal disc is vertically and slidably arranged on the inner wall of the sleeve disc, an adjusting pipe is rotatably arranged at the bottom of the water removal disc, the adjusting pipe is positioned in a gap between the stirring pipe and the fixed ring and is attached to the stirring pipe and the fixed ring, and a spring sleeved on the adjusting pipe is further connected between the water removal disc and the fixed ring;
the pressure control assembly is used for controlling the air pressure in the stirring pipe, so that the liquid level in the stirring pipe can be intermittently raised, and the liquid level can overflow through the liquid inlet of the detection assembly;
and the switching assembly is used for switching the internal communication between the detection assembly and the stirring pipe.
Preferably, the pressure control assembly comprises a conversion box connected to the top end of the stirring pipe, the conversion box is located in the sleeve disc and the water removal disc, the top of the conversion box is rotationally connected with the tank cover through a connecting rod, a piston block is slidably mounted on the inner wall of the conversion box, sliding rods penetrating out of the conversion box are fixed on two sides of the piston block, the end portions of the sliding rods are in rolling contact with the inner wall of the water removal disc through rollers, unidirectional outlets for unidirectional discharging of gas or liquid are formed in two side walls of the conversion box, a unidirectional valve for enabling the gas or liquid to enter the conversion box is mounted in the stirring pipe close to the conversion box, a hollow hole is formed in the outer wall of the adjusting pipe between the water removal disc and the fixing ring, a leakage hole is formed in the position of the stirring pipe close to the hollow hole, an outer communicating groove capable of being communicated with a liquid inlet of the detection assembly is formed in the outer wall of the stirring pipe, and a leakage hole is formed in the inner connecting groove communicated with the outer communicating groove.
Preferably, the switching assembly comprises a plurality of groups of switching grooves formed in the outer wall of the adjusting pipe, the switching grooves are connected end to end, the number of the switching grooves corresponds to that of the detecting assembly one by one, each switching groove comprises a vertical groove and a chute which are communicated with each other, an elastic telescopic rod inserted into the vertical groove or the chute is arranged at the inner ring of the fixing ring, a height difference is arranged between the vertical groove and the chute, and the elastic telescopic rod can only slide along one direction.
Preferably, the detection component comprises a plurality of drainage tubes which are distributed in an annular shape and are communicated with the extension tube, a detection tank is arranged at the tail end of the drainage tube, a containing bottle for containing detection reagent is arranged inside the detection tank, the detection tank and the containing bottle are all arranged in a transparent mode, and a detector for monitoring the condition in the containing bottle is further arranged at the inner bottom of the detection tank.
Preferably, a through groove is formed in the inner bottom of the water removal disc, a filter screen is fixed on the inner wall of the through groove, an electric shielding plate capable of rotating to open the filter screen is further installed on the inner wall of the through groove, and the electric shielding plate is connected with the detector through an electric signal.
Preferably, the drainage tube is obliquely arranged downwards in an inclined mode, and the detection tank is connected with the drainage tube through threads.
Preferably, an inner conical surface is arranged at the communication part of the drainage tube and the extension tube.
Preferably, the bottom of the ball milling tank further comprises a liquid discharge pipe, and an electromagnetic valve is arranged on the liquid discharge pipe.
Preferably, the sleeve disc is in sliding connection with the water removal disc through a flat key, and the length of the flat key is longer than the distance between the water removal disc and the fixed ring.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the sampling assembly is used for intermittently sampling from the ball milling tank, and the sample is injected into the detection assembly to detect the content of sodium hydroxide, so that whether the sodium hydroxide and the detection assembly react completely can be accurately known, the time for carrying out the water removal process can be accurately controlled, and the quality of the finally prepared sodium ethoxide solution can be improved.
Drawings
FIG. 1 is a schematic perspective view of the present invention;
FIG. 2 is a front cross-sectional view of the present invention;
FIG. 3 is a cross-sectional view taken along line A-A of FIG. 2 in accordance with the present invention;
FIG. 4 is a cross-sectional perspective view of the present invention;
FIG. 5 is a perspective view of a regulator tube of the present invention;
FIG. 6 is a partial cutaway perspective view of a milling pot of the present invention;
FIG. 7 is a front view of the present invention;
fig. 8 is a cross-sectional view taken along line B-B of fig. 7 in accordance with the present invention.
In the figure: 1. a ball milling tank; 2. a can lid; 3. a stirring tube; 4. a sleeve disk; 5. a water removal disc; 6. an adjusting tube; 7. a spring; 8. a fixing ring; 9. a drainage tube; 10. a detection tank; 11. an inner communication groove; 12. an outer communication groove; 13. a stirring rod; 14. an elastic telescopic rod; 15. a vertical groove; 16. a chute; 17. routing holes; 18. a leakage hole; 19. a holding bottle; 20. a detector; 21. a filter screen; 22. a transfer box; 23. a piston block; 24. a slide bar; 25. a unidirectional outlet; 26. a through groove; 27. an electric shielding plate; 28. a liquid discharge pipe; 29. and a vent hole.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1 to 8, the present invention provides a technical solution: a production system for sodium ethoxide, including ball-milling jar 1, steel ball and can fix the cover 2 at ball-milling jar 1 open-top department, still include:
a rotatable stirring pipe 3 arranged at the bottom of the tank cover 2, and a plurality of stirring rods 13 are fixed at the lower half section of the stirring pipe 3;
the stirring pipe 3 passes through the inner ring of the fixed ring 8, an extension pipe is coaxially fixed at the bottom of the fixed ring 8, a plurality of annularly distributed detection components are arranged on the outer wall of the extension pipe, and the detection components are used for detecting the content of sodium hydroxide;
and the sampling assembly is used for intermittently sampling from the ball milling tank 1 and sequentially injecting the samples collected before and after into different detection assemblies for content detection.
In the examples, a ball milling process was used to produce sodium ethoxide, as follows:
placing anhydrous ethanol and sodium hydroxide raw materials which are prepared in proportion and steel balls in a ball milling tank 1 together, fixing a tank cover 2 at the top of the ball milling tank 1, and driving a stirring pipe 3 to rotate by using an external mechanism such as a motor and the like to enable reactants to generate sodium ethoxide under the action of ball milling;
wherein, the ball milling tank 1 comprises a self-contained cold water jacket, and in the reaction process, the generated heat is taken away through the circulation of cooling liquid in the cold water jacket so as to reduce the temperature of reactants in the ball milling tank 1;
in the reaction process, intermittently sampling, namely, sampling at fixed time, from the ball milling tank 1 through a sampling assembly, and injecting the sample into a detection assembly to detect the content of sodium hydroxide, wherein if the detection assembly detects that sodium hydroxide exists in the sample solution, the reaction is not completed;
otherwise, if the detection component does not detect sodium hydroxide, the reaction of the sample and the reactant in the ball milling tank 1 is finished, and the sodium ethoxide solution and water generated by the reaction are in the ball milling tank 1, so that the subsequent water removal process can be carried out;
therefore, whether the sodium hydroxide and the reactant are completely reacted can be accurately known through detecting the content of the sodium hydroxide in the reactant, so that the time for carrying out the water removal process can be accurately controlled, and the quality of the finally prepared sodium ethoxide solution can be improved.
The sampling assembly comprises a sleeve disc 4 eccentrically fixed at the bottom of the tank cover 2, a water removal disc 5 is vertically and slidably arranged on the inner wall of the sleeve disc 4, an adjusting pipe 6 is rotatably arranged at the bottom of the water removal disc 5, the adjusting pipe 6 is positioned in a gap between the stirring pipe 3 and the fixed ring 8 and is attached to the stirring pipe 3 and the fixed ring 8, and a spring 7 sleeved on the adjusting pipe 6 is further connected between the water removal disc 5 and the fixed ring 8;
the pressure control assembly is used for controlling the air pressure in the stirring pipe 3, so that the liquid level in the stirring pipe 3 can be intermittently raised, and the liquid level can overflow through the liquid inlet of the detection assembly;
and the switching component is used for switching the internal communication between the detection component and the stirring pipe 3.
In the process of rotating the stirring pipe 3, one of the detection components is communicated with the inside of the stirring pipe 3 through the switching component, so that the air pressure in the stirring pipe 3 is controlled through the pressure control component, the liquid level of reactants in the stirring pipe 3 can be controlled, and when the air pressure in the stirring pipe 3 is reduced, the liquid level in the stirring pipe 3 can rise until the liquid level passes through the liquid inlet of the detection component and then enters the detection component for detection;
then the pressure control assembly enables the air pressure in the stirring tube 3 to be normal, the liquid level in the stirring tube 3 is reduced at the moment, the liquid level can be intermittently increased through continuous adjustment of the air pressure by the pressure control assembly, and then reactants in the stirring tube 3 can enter different detection assemblies successively through switching of the detection assemblies until the detection assemblies do not detect the content of sodium hydroxide, so that the effect of timing sampling detection is achieved.
Embodiments of the pressure control assembly are described with particular reference to fig. 3-4;
the pressure control assembly comprises a conversion box 22 connected to the top end of the stirring pipe 3, the conversion box 22 is located in the sleeve disc 4 and the water removal disc 5, the top of the conversion box 22 is rotationally connected with the tank cover 2 through a connecting rod, a piston block 23 is slidably mounted on the inner wall of the conversion box 22, sliding rods 24 penetrating out of the conversion box 22 are fixed on two sides of the piston block 23, the end portions of the sliding rods 24 are in rolling contact with the inner wall of the water removal disc 5 through rollers, unidirectional outlets 25 for unidirectional discharge of gas or liquid are formed in two side walls of the conversion box 22, a unidirectional valve for enabling the gas or liquid to enter the conversion box 22 is mounted in the stirring pipe 3 close to the conversion box 22, a hollow hole 17 is formed in the outer wall of the adjusting pipe 6 located between the water removal disc 5 and the fixed ring 8, a leakage hole 18 is formed in the position of the stirring pipe 3 close to the hollow hole 17, an outer communication groove 12 capable of being communicated with a liquid inlet of the detection assembly is formed in the outer wall of the stirring pipe 3, an inner communication groove 11 capable of being communicated with the outer communication groove 12 is formed in the inner wall of the water removal disc 5, and a leakage hole 29 is formed in the inner wall of the water removal disc 5.
As can be seen from the above, the stirring tube 3 is driven by the motor to rotate continuously, so that the conversion box 22 rotates in the sleeve disc 4, and the sleeve disc 4 and the tank cover 2 are eccentrically arranged, namely, the sleeve disc 4 and the stirring tube 3 are eccentrically arranged, so that the roller at the end of the sliding rod 24 is continuously contacted with the inner wall of the water removal disc 5 along with the rotation of the conversion box 22, and the piston block 23 is driven to slide in the conversion box 22 in a reciprocating manner, and air in the stirring tube 3 is continuously filled into the sleeve disc 4 while sliding in a reciprocating manner, so that a negative pressure state is formed in the stirring tube 3;
with the filling of air, the water removal disc 5 moves downwards under the action of internal air pressure, the adjusting pipe 6 releases the sealing of the air leakage hole 18 under the action of the hollow hole 17, the air inlet of the air leakage hole 18 can effectively slow down the negative pressure enhancement speed in the stirring pipe 3, and finally the liquid level in the stirring pipe 3 can slowly rise, so that the unreacted complete reactant is prevented from being directly sucked into the water removal disc 5;
along with the continuous rotation of the conversion box 22, the negative pressure in the stirring tube 3 is gradually increased, and the liquid level is gradually increased until the liquid level overflows through the liquid inlet of the detection assembly, namely, the solution can enter the detection assembly through the inner communication groove 11 and the outer communication groove 12, and the preliminary pressure regulating process is completed;
meanwhile, the air pressure in the water removing disc 5 and the sleeve disc 4 is gradually increased, the water removing disc 5 also continuously drives the regulating tube 6 to move downwards, when the liquid level overflows the detection assembly and enters from the liquid inlet, the continuous downwards movement of the water removing disc 5 can enable the air release hole 29 to be communicated with the outside, meanwhile, the outer communication groove 12 formed in the regulating tube 6 is communicated with the ball milling tank 1, the air release hole 29 can be used for releasing the pressure in the water removing disc 5 and the sleeve disc 4, the water removing disc 5 is reset under the action of the spring 7, and the inner communication groove 11 can be used for releasing the negative pressure state in the stirring tube 3 due to the communication of the outer communication groove 12, so that the air pressure in the stirring tube 3 is recovered, and meanwhile, the liquid level can also fall;
then the switching component is switched to be communicated with the next detecting component and the stirring pipe 3, and the process is repeated to finish the secondary sampling detection, so that the sampling detection process can be automatically finished through the change of the air pressure in the stirring pipe 3.
Embodiments of the switching assembly can be seen with particular reference to fig. 4 and 5;
the switching assembly comprises a plurality of groups of switching grooves formed in the outer wall of the adjusting pipe 6, the switching grooves are connected end to end, the number of the switching grooves corresponds to that of the detecting assembly one by one, each switching groove comprises a vertical groove 15 and a chute 16 which are communicated with each other, an elastic telescopic rod 14 which is inserted into the vertical groove 15 or the chute 16 is arranged at the inner ring of the fixed ring 8, a height difference is arranged in the vertical groove 15 and the chute 16, and the elastic telescopic rod 14 can only slide along one direction.
As can be seen from the above description, the switching assembly switches after the air pressure in the stirring tube 3 is recovered, in the process of pressure regulation, that is, the water removal disc 5 drives the regulating tube 6 to move downwards, the elastic telescopic rod 14 slides in the vertical groove 15, meanwhile, the limiting effect of the elastic telescopic rod 14 on the vertical groove 15 can ensure that the regulating tube 6 cannot rotate in the process, so that the outer communicating groove 12 on the regulating tube is communicated with the liquid inlet of the detecting assembly, and the inner communicating groove 11 formed in the inner wall of the stirring tube 3 is intermittently communicated with the outer communicating groove 12 when the stirring tube rotates, so that the inner communicating groove is intermittently communicated with the detecting assembly;
then when the air pressure in the stirring tube 3 is recovered, namely, when the water removal disc 5 moves upwards under the action of the spring 7, the adjusting tube 6 also moves upwards, and at the moment, the elastic telescopic rod 14 slides along the chute 16, so that the adjusting tube 6 rotates for a certain angle, and the outer communication groove 12 is communicated with the next detection assembly, thereby achieving the purpose of switching the detection assemblies;
therefore, the switching of the detection assembly can be automatically completed through the change of air pressure every time, and the effect of automatic detection is achieved.
The rotation direction of the stirring tube 3 is preferably opposite to that of the adjusting tube 6, so that the stirring tube 3 can be prevented from driving the adjusting tube 6 to rotate together under the limiting action of the vertical groove 15.
An embodiment of the detection assembly is shown in particular in fig. 4;
the detection component comprises a plurality of drainage tubes 9 which are distributed in an annular shape and are communicated with the extension tube, a detection tank 10 is installed at the tail end of the drainage tube 9, a containing bottle 19 for containing detection reagent is arranged inside the detection tank 10, the detection tank 10 and the containing bottle 19 are both arranged in a transparent mode, and a detector 20 for monitoring the condition in the containing bottle 19 is further installed at the inner bottom of the detection tank 10.
Before production and processing, pouring a detection reagent into the containing bottle 19, and detecting sodium hydroxide in the reactant by using a back titration mode, wherein the detection reagent adopts a copper sulfate solution;
since copper sulfate reacts with sodium hydroxide to form copper hydroxide precipitate and sodium sulfate, while absolute ethyl alcohol is an organic matter and copper sulfate is an inorganic salt, the absolute ethyl alcohol does not react with copper sulfate under the condition of no catalyst or high-temperature environment, the same sodium ethoxide is sodium salt of ethanol, and sodium ethoxide needs to react with copper sulfate under the acidic environment, so that after a sample solution is dripped into the containing bottle 19, whether copper hydroxide precipitate is generated in the containing bottle 19 or not can be detected by the detector 20, whether sodium hydroxide residue exists in the sample solution or not can be detected, and if the residue indicates that the reaction is not complete, the reaction is complete.
It is worth mentioning that the color change occurs when sodium hydroxide reacts with copper sulfate, the solution gradually changes from light blue to colorless along with the reaction of copper sulfate, and meanwhile, blue copper hydroxide precipitation is generated, and the specific change degree is related to the residual quantity of sodium hydroxide, so that the detection purpose can be achieved through color monitoring.
After detecting that the reaction in the ball milling tank 1 is complete, referring to fig. 3 and 6, for an embodiment of removing water from the sodium ethoxide solution;
the inner bottom of the water removal disc 5 is provided with a through groove 26, a filter screen 21 is fixed on the inner wall of the through groove 26, an electric shielding plate 27 capable of rotating to open the filter screen 21 is further arranged on the inner wall of the through groove 26, and the electric shielding plate 27 is connected with the detector 20 through an electric signal.
When the detector 20 does not detect the precipitate in the detection process, it indicates that the reaction in the ball milling tank 1 is complete, at this time, the detector 20 controls the electric shielding plate 27 to slide in the through groove 26 through an electric signal, the filter screen 21 is opened, and calcium oxide or magnesium oxide is stored in the water removal disc 5 in advance, so that after the filter screen 21 is opened, the water removal disc 5 and the sleeve disc 4 are communicated with the outside, the water removal disc 5 is not moved downwards by the conversion box 22 when the stirring tube 3 rotates, the air leakage hole 18 is not communicated with the hollow hole 17, a good sealing environment is kept by the stirring tube 3, so that the sodium ethoxide solution after the reaction in the ball milling tank 1 is sucked into the water removal disc 5 by the reciprocating sliding of the piston block 23 along with the rotation of the conversion box 22, the water is reacted to generate the precipitate by calcium oxide, the water in the sodium ethoxide solution is removed, and the sodium ethoxide solution falls back into the ball milling tank 1 through the filter screen 21;
thus, along with the continuous rotation of the stirring tube 3, the sodium ethoxide solution can form an internal circulation state, in the circulation process, the calcium oxide is utilized to remove water, meanwhile, the continuous circulation of sodium ethoxide can also avoid the overlong contact time of the sodium ethoxide solution and generated calcium hydroxide, thus not only ensuring the water removal efficiency, but also reducing the influence on the sodium ethoxide solution, and the continuous circulation of the sodium ethoxide solution can also improve the contact with the calcium oxide so as to accelerate the reaction of the water and the calcium oxide and improve the water removal efficiency, and the rotation of the stirring tube 3 can be stopped until no precipitate is formed;
therefore, after the completion of the reaction in the ball milling tank 1 is detected, the sodium ethoxide solution can be immediately subjected to water removal treatment, and the quality of the sodium ethoxide solution can be further effectively improved.
It should be noted that the shapes of the through groove 26, the filter screen 21 and the electric shielding plate 27 are not limited, and the arc surface is designed to prevent the sodium ethoxide solution from dripping on the fixing ring 8 when falling down, and other shapes can be designed according to practical situations.
In one of the preferred embodiments, the drainage tube 9 is obliquely arranged downwards, and the detection tank 10 is connected with the drainage tube 9 through threads.
The inclined arrangement of the drainage tube 9 can ensure that the solution can enter the detection tank 10, and meanwhile, the flow of the sodium ethoxide solution in the stirring tube 3 can not bring out the drainage tube 9 and the solution in the detection tank 10 in the subsequent water removal process, so that the sodium ethoxide solution is prevented from being polluted.
The bottom of the ball milling tank 1 also comprises a liquid discharge pipe 28, and an electromagnetic valve is arranged on the liquid discharge pipe 28.
After the water removal process is completed, the sodium ethoxide solution may be discharged from the drain pipe 28 by opening the electromagnetic valve.
An inner conical surface is arranged at the communication part of the drainage tube 9 and the extension tube.
The solution in the drainage tube 9 can be further ensured to be reversely led out by arranging the inner conical surface, so that the pollution to the sodium ethoxide solution is avoided.
The sleeve disk 4 is in sliding connection with the water removal disk 5 through a flat key, and the length of the flat key is longer than the distance between the water removal disk 5 and the fixed ring 8.
The standard components used in the present embodiment may be purchased directly from the market, and the nonstandard structural components according to the descriptions of the specification and the drawings may also be obtained directly by unambiguous processing according to the common general knowledge in the prior art, and meanwhile, the connection manner of each component adopts the conventional means mature in the prior art, and the machinery, the components and the equipment all adopt the conventional types in the prior art, so that the specific description will not be made here.
Claims (6)
1. The utility model provides a production system for sodium ethoxide, includes ball-milling jar (1), steel ball and can fix cover (2) at ball-milling jar (1) open-top department, its characterized in that still includes:
the stirring pipe (3) is arranged at the bottom of the tank cover (2) and can rotate, and a plurality of stirring rods (13) are fixed at the lower half section of the stirring pipe (3);
the stirring pipe (3) penetrates through the inner ring of the fixed ring (8), an extension pipe is coaxially fixed at the bottom of the fixed ring (8), a plurality of annularly distributed detection assemblies are arranged on the outer wall of the extension pipe, and the detection assemblies are used for detecting the content of sodium hydroxide;
the sampling assembly is used for intermittently sampling from the ball milling tank (1), and sequentially injecting samples collected before and after into different detection assemblies for detection;
the sampling assembly comprises a sleeve disc (4) eccentrically fixed at the bottom of the tank cover (2), a water removal disc (5) is vertically and slidably arranged on the inner wall of the sleeve disc (4), an adjusting pipe (6) is rotatably arranged at the bottom of the water removal disc (5), the adjusting pipe (6) is positioned in a gap between the stirring pipe (3) and the fixed ring (8) and is attached to the stirring pipe (3) and the fixed ring (8), and a spring (7) sleeved on the adjusting pipe (6) is further connected between the water removal disc (5) and the fixed ring (8);
the pressure control assembly is used for controlling the air pressure in the stirring pipe (3), so that the liquid level in the stirring pipe (3) can be intermittently raised, and the liquid level can overflow through the liquid inlet of the detection assembly;
the switching component is used for switching the internal communication between the detection component and the stirring pipe (3);
the pressure control assembly comprises a conversion box (22) connected to the top end of a stirring pipe (3), the conversion box (22) is positioned in a sleeve disc (4) and a water removal disc (5), the top of the conversion box (22) is rotationally connected with a tank cover (2) through a connecting rod, piston blocks (23) are slidably mounted on the inner wall of the conversion box (22), slide rods (24) penetrating out of the conversion box (22) are fixed on two sides of the piston blocks (23), the ends of the slide rods (24) are in rolling contact with the inner wall of the water removal disc (5) through rollers, unidirectional outlets (25) for unidirectional discharge of gas or liquid are formed in two side walls of the conversion box (22), a unidirectional valve for enabling the gas or liquid to enter the conversion box (22) in a unidirectional mode is arranged in the interior of the stirring pipe (3) close to the conversion box (22), a hollow hole (17) is formed in the outer wall of a pipe (6) between the water removal disc (5) and a fixed ring (8), a position of the stirring pipe (3) close to the hollow hole (17) is provided with a drain hole (18), a detection groove (12) can be formed in the inner wall of the stirring pipe (3), the detection groove (12) can be communicated with the outer wall of the stirring pipe (12), the inner wall of the water removal disc (5) is also provided with a gas leakage hole (29);
the switching assembly comprises a plurality of groups of switching grooves which are formed in the outer wall of the adjusting pipe (6), the switching grooves are connected end to end, the number of the switching grooves corresponds to that of the detecting assembly one by one, each switching groove comprises a vertical groove (15) and a chute (16) which are communicated with each other, an elastic telescopic rod (14) which is inserted into the vertical groove (15) or the chute (16) is arranged at the inner ring of the fixed ring (8), height differences are arranged in the vertical groove (15) and the chute (16), and the elastic telescopic rod (14) can only slide along one direction;
the detection assembly comprises a plurality of drainage tubes (9) which are distributed in an annular mode and are communicated with the extension tubes, a detection tank (10) is arranged at the tail end of each drainage tube (9), a containing bottle (19) for containing detection reagents is arranged inside each detection tank (10), the detection tank (10) and the containing bottle (19) are all arranged in a transparent mode, and a detector (20) for monitoring conditions in the corresponding containing bottle (19) is further arranged at the inner bottom of each detection tank (10).
2. The production system for sodium ethoxide according to claim 1, wherein: the inner bottom of the water removal disc (5) is provided with a through groove (26), a filter screen (21) is fixed on the inner wall of the through groove (26), an electric shielding plate (27) capable of rotating to open the filter screen (21) is further arranged on the inner wall of the through groove (26), and the electric shielding plate (27) is connected with the detector (20) through an electric signal.
3. The production system for sodium ethoxide according to claim 1, wherein: the drainage tube (9) is obliquely downwards arranged, and the detection tank (10) is connected with the drainage tube (9) through threads.
4. The production system for sodium ethoxide according to claim 1, wherein: an inner conical surface is arranged at the communication part of the drainage tube (9) and the extension tube.
5. The production system for sodium ethoxide according to claim 1, wherein: the bottom of the ball milling tank (1) further comprises a liquid discharge pipe (28), and an electromagnetic valve is arranged on the liquid discharge pipe (28).
6. The production system for sodium ethoxide according to claim 1, wherein: the sleeve disc (4) is in sliding connection with the water removal disc (5) through a flat key, and the length of the flat key is longer than the distance between the water removal disc (5) and the fixing ring (8).
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| CN202410019000.XA CN117505005B (en) | 2024-01-05 | 2024-01-05 | Production system for sodium ethoxide |
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| JP2006206578A (en) * | 2004-12-28 | 2006-08-10 | Mitsubishi Chemicals Corp | Method for producing amine compound, electrophotographic photoreceptor having photosensitive layer containing the amine compound, cartridge having the photoreceptor and image formation apparatus |
| CN106045813A (en) * | 2016-01-04 | 2016-10-26 | 武汉理工大学 | Ball milling method for preparation of sodium ethoxide |
| FR3056576A1 (en) * | 2016-09-29 | 2018-03-30 | Easyl | PROCESS FOR PRODUCING CALCIUM DIGLYCEROXIDE |
| CN115645952A (en) * | 2022-11-15 | 2023-01-31 | 天津市圣融祺科技发展有限公司 | Method and system for producing sodium ethoxide |
| CN117003616A (en) * | 2023-08-01 | 2023-11-07 | 山东金柯工程设计有限公司 | Sodium ethoxide production process |
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| EP2184109B1 (en) * | 2007-07-06 | 2017-08-23 | M Technique Co., Ltd. | Method for producing nanoparticles by forced ultra-thin film rotary processing |
| WO2009035019A1 (en) * | 2007-09-12 | 2009-03-19 | M.Technique Co., Ltd. | Ultrafine particles of titanium dioxide and process for producing the ultrafine particles |
| US11169128B2 (en) * | 2018-04-16 | 2021-11-09 | Chinese Academy Of Inspection And Quarantine | Electronic ID database and detection method for pesticide compound in edible agro-products based on LC-Q-Orbitrap |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006206578A (en) * | 2004-12-28 | 2006-08-10 | Mitsubishi Chemicals Corp | Method for producing amine compound, electrophotographic photoreceptor having photosensitive layer containing the amine compound, cartridge having the photoreceptor and image formation apparatus |
| CN106045813A (en) * | 2016-01-04 | 2016-10-26 | 武汉理工大学 | Ball milling method for preparation of sodium ethoxide |
| FR3056576A1 (en) * | 2016-09-29 | 2018-03-30 | Easyl | PROCESS FOR PRODUCING CALCIUM DIGLYCEROXIDE |
| CN115645952A (en) * | 2022-11-15 | 2023-01-31 | 天津市圣融祺科技发展有限公司 | Method and system for producing sodium ethoxide |
| CN117003616A (en) * | 2023-08-01 | 2023-11-07 | 山东金柯工程设计有限公司 | Sodium ethoxide production process |
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