CN114210292A - Preparation method and equipment of electronic-grade hexamethyldisilazane - Google Patents
Preparation method and equipment of electronic-grade hexamethyldisilazane Download PDFInfo
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- CN114210292A CN114210292A CN202111488322.1A CN202111488322A CN114210292A CN 114210292 A CN114210292 A CN 114210292A CN 202111488322 A CN202111488322 A CN 202111488322A CN 114210292 A CN114210292 A CN 114210292A
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- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 105
- 239000000463 material Substances 0.000 claims abstract description 68
- 238000003756 stirring Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 34
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims abstract description 32
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 26
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000005051 trimethylchlorosilane Substances 0.000 claims abstract description 16
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000004519 grease Substances 0.000 claims abstract description 8
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 230000001105 regulatory effect Effects 0.000 claims description 41
- 238000003860 storage Methods 0.000 claims description 39
- 230000006698 induction Effects 0.000 claims description 8
- 150000003863 ammonium salts Chemical class 0.000 claims description 6
- 150000007522 mineralic acids Chemical class 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 238000011897 real-time detection Methods 0.000 description 2
- 238000002444 silanisation Methods 0.000 description 2
- 229930186147 Cephalosporin Natural products 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 229940124587 cephalosporin Drugs 0.000 description 1
- 150000001780 cephalosporins Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The application discloses a preparation method of electronic-grade hexamethyldisilazane, which comprises the following steps: the method comprises the following steps: s1, preparing materials, namely preparing certain amounts of trimethylchlorosilane, carbonate, hexamethyldisiloxane and sulfuric acid, wherein the weight part ratio of the trimethylchlorosilane to the carbonate to the hexamethyldisiloxane is 100: 50-90: 30-180; s2: the preliminary reaction, adding the measured carbonate and hexamethyldisiloxane into a reaction kettle, stirring, adding trimethylchlorosilane into the reaction kettle for reaction, cooling the mixed liquid after the reaction is stopped, and obtaining high-purity hexamethyldisiloxane through centrifugal separation after cooling; s3: comprehensive reaction, namely mixing and reacting metered hexamethyldisiloxane and sulfuric acid, and removing the sulfuric acid by a standing method after the reaction to obtain silicone grease; s4: and (3) preparing a finished product, adding the silicone grease into the pressure kettle, adding benzene, mixing and stirring, and continuously introducing ammonia gas for reaction in the stirring process.
Description
Technical Field
The invention belongs to the field of organic chemistry, and particularly relates to a method and equipment for preparing electronic-grade hexamethyldisilazane.
Background
Hexamethyldisilazane (HMDS) is an important medical intermediate, is mainly used as a silanization reagent for silanization protection of amino acid, carboxylic acid, alcohol and amide, and is widely applied to synthesis of cephalosporin antibiotics in particular. For a long time, two main methods for producing Hexamethyldisilazane (HMDS) have been proposed: firstly, the method is described in US4622076 and CN200580035277, which uses trimethylchlorosilane to react with liquid ammonia in a large amount of organic solvent under certain pressure and temperature to directly generate Hexamethyldisilazane (HMDS) and by-product ammonium chloride; secondly, in U.S. Pat. No. 4,430,5427, a process for preparing alkylsilylamine by reacting trialkylhydrosilane with liquid ammonia is described, wherein the alkylhydrogensilane is not of much practical value in the industry at present, since it is expensive.
In the course of working, often adopt reation kettle to advance processing, but in the course of working, most all adopt manual joining, from the feed inlet on the reation kettle cover, toward the internal raw materials that adds of cauldron, whole in-process, not only intensity of labour is great, and is inefficient moreover, and manual still leads to the proportion of adding inaccurate easily, influences the reaction, still needs the enhancement.
Disclosure of Invention
The invention aims to provide a method and equipment for preparing electronic-grade hexamethyldisilazane, which can solve the problems.
The application aims to provide a preparation method of electronic-grade hexamethyldisilazane, which comprises the following steps: the method comprises the following steps: s1, preparing materials, namely preparing certain amounts of trimethylchlorosilane, carbonate, hexamethyldisiloxane and sulfuric acid, wherein the weight part ratio of the trimethylchlorosilane to the carbonate to the hexamethyldisiloxane is 100: 50-90: 30-180; s2: the preliminary reaction, adding the measured carbonate and hexamethyldisiloxane into a reaction kettle, stirring, adding trimethylchlorosilane into the reaction kettle for reaction, cooling the mixed liquid after the reaction is stopped, and obtaining high-purity hexamethyldisiloxane through centrifugal separation after cooling; s3: comprehensive reaction, namely mixing and reacting metered hexamethyldisiloxane and sulfuric acid, and removing the sulfuric acid by a standing method after the reaction to obtain silicone grease; s4: and (3) preparing a finished product, adding the silicone grease into the pressure kettle, adding benzene, dissolving and stirring, continuously introducing ammonia gas during stirring to react to generate hexamethyldisilazane and ammonium salt, and centrifuging to remove the ammonium salt to obtain the hexamethyldisilazane.
Further, the mole ratio of the hexamethyldisiloxane to the inorganic acid is 1: 0.6-0.85 or 1: 4-18.
Further: in S2, the trimethylchlorosilane is dropped into the carbonate, the hexamethyldisiloxane, and the mixed solution in a dropping manner.
Furthermore, the invention also discloses production equipment of the electronic-grade hexamethyldisilazane, which comprises a reaction kettle, wherein the reaction kettle comprises a kettle body, a kettle cover arranged on the kettle body, and a stirring device arranged in the kettle body, the reaction kettle further comprises a feeding device, and the feeding device comprises: the reaction kettle is arranged in the reaction kettle, a first storage tank is used for storing reaction materials, a first feeding pipe is arranged between the first storage tank and the reaction kettle, a first feeding pipe is further arranged on the first storage tank, and a first pump is further arranged on the first feeding pipe; the second storage tank is used for storing materials for reaction, a second feeding pipe is arranged between the second storage tank and the reaction kettle, a second feeding pipe is further arranged on the second storage tank, and a second pump is further arranged on the second feeding pipe; the device comprises a first pump, a second pump, a control device and a controller, wherein the first pump and the second pump are connected with the control device and control the first pump and the second pump, and the control device can control the first pump and the second pump to convey reaction materials with corresponding numerical values according to input proportioning values required by reaction by inputting the proportioning values required by the reaction.
Through being equipped with controlling means, can control first pump and second pump, when needs react, ratio input controlling means between the material that the staff will need to react, thereby controlling first pump and second pump and carrying the material for the reaction of corresponding numerical value according to the ratio of input through the required ratio of input reaction of controlling means, first bin and second bin are used for storing the material for the reaction, the bin can increase according to the promotion of reaction needs material kind, come to control and can add the reaction material to reation kettle in the automation through being equipped with controlling means, needn't artifical the interpolation, and whole process all goes on under encapsulated situation, can improve the quality and the efficiency of reaction, and simultaneously, can also improve the accuracy of reaction.
Further, the control device includes: the first controller comprises a first regulating valve connected with the first pump, and the first regulating valve is arranged on the first feeding pipe; the second controller comprises a second regulating valve connected with the second pump, and the second regulating valve is arranged on the second feeding pipe; the first controller controls the first regulating valve to operate, the first controller is connected with the second controller and controls the second controller to operate, the first controller controls the first regulating valve to operate according to a set proportioning value, meanwhile, the first controller controls the second controller to operate, and the second controller controls the second regulating valve to operate according to a command sent by the first controller and according to the set proportioning value.
The first controller can also control the second controller to operate when controlling the operation of the first regulating valve, the second controller controls the operation of the second regulating valve according to the command sent by the first controller and the set proportioning value, the process of conveying different reaction materials by the first pump and the second pump is detected and corrected in real time by adopting the operation mode, and therefore the accuracy of the proportion between different materials is ensured to react according to the proportioning value input by a user strictly.
Further, the control device further comprises an adjusting device, and the adjusting device comprises: the flowmeter is arranged on the first feeding pipe and used for detecting and feeding back the flow of the first pump; the comparison device is connected with the flowmeter and used for receiving a flow numerical value fed back by the flowmeter, comparing the flow numerical value with a set proportioning value to obtain a comparison signal and then sending the obtained comparison signal to the first controller; the first controller controls the first regulating valve to operate and controls the second controller to operate according to a comparison signal sent by the comparison device, and the second controller regulates the flow of the second regulating valve according to the comparison signal sent by the first controller and according to a set proportioning value.
The adjusting device is arranged, so that the control of the first adjusting valve and the second adjusting valve can be more accurate, the flowmeter detects the flow of the first pump during adjustment, namely, the first storage tank inputs the numerical value reflecting the material into the reaction kettle, the detected numerical value is transmitted to the comparison device, the comparison device compares the value with a set proportioning value to obtain a comparison signal, and then sends the obtained comparison signal to the first controller, the first controller controls the operation of the first regulating valve and controls the operation of the second controller according to the comparison signal sent by the comparison device, the second controller adjusts the flow of the second regulating valve according to the comparison signal sent by the first controller and the set proportioning value, therefore, the influence of errors can be effectively reduced, the proportioning precision among the reaction materials is improved, and the problem of inaccurate ratio when the reaction materials are added is effectively prevented.
Further, be equipped with first liquid level induction system in the first bin, be equipped with second liquid level induction system in the second bin, still be equipped with the third governing valve on the first inlet pipe, can be equipped with the fourth governing valve on the second inlet pipe, just first liquid level induction system, second liquid level induction system, third governing valve and fourth governing valve all are connected with first controller.
In the use process, when the first liquid level sensing device detects that the liquid level of the reaction material stored in the first storage tank is lower than the set lowest liquid level, the first controller controls the third regulating valve to open, and the reaction material is injected into the first storage tank from the first feeding pipe until the liquid level in the first storage tank reaches the set highest liquid level; when the second liquid level sensing device detects that the liquid level of the reaction material stored in the second storage box is lower than the set lowest liquid level, the first controller controls the fourth regulating valve to open, the reaction material is injected into the second storage box from the second feeding pipe until the liquid level in the second storage box reaches the set highest liquid level, the material can be automatically added, the processing time is saved, and the processing efficiency is improved.
Further, the stirring device includes: a stirring shaft; one end of the stirring shaft is provided with a driving motor for driving the stirring shaft to rotate; the stirring blades are spirally arranged on the stirring shaft, two stirring blades are symmetrically arranged on the stirring shaft, and the spiral directions of the two stirring blades are opposite; wherein, stirring vane's blade surface orientation the axis direction of the cauldron body, two stirring vane's both ends all are equipped with parallel blade, parallel blade's the other end with stirring shaft connection.
Set up stirring vane on the (mixing) shaft with helical gear, when preventing that the material in the reaction cauldron stirs, the reaction material forms the material circulation in the outside and the inside of the spiral that helical blade formed, the reaction material that is located the spiral outside upwards flows under helical blade's effect, simultaneously, the material that is located the internal top of cauldron gets into the spiral inside back downwards flow to form the material circulation, the material mixes with higher speed, the material mixing effect homogeneous that makes the internal different positions of cauldron, product quality has effectively been improved.
The invention has the beneficial effects that:
1. the control device is arranged, so that a worker inputs a ratio value between materials to be reacted into the control device, the control device can control the first pump and the second pump to convey reaction materials with corresponding numerical values according to the input ratio value by inputting the ratio value required by reaction, the first storage tank and the second storage tank are used for storing the reaction materials, and the number of the storage tanks can be increased according to the promotion of the types of the materials required by the reaction;
2. the control device is arranged for controlling, so that the reaction materials can be automatically added into the reaction kettle without manual addition, the whole process is carried out in a sealed state, the quality and the efficiency of the reaction can be improved, and the reaction accuracy can be improved;
3. the first controller can control the first regulating valve to operate and also can control the second controller to operate at the same time, the second controller controls the second regulating valve to operate according to a command sent by the first controller and a set proportioning value, and the operation mode is adopted to realize real-time detection and correction of the process of conveying different reaction materials by the first pump and the second pump, so that the accuracy of the proportion between different materials is ensured to react according to the proportioning value input by a user strictly and the qualification rate;
4. the flowmeter detects the flow of first pump, the numerical value that will detect is transmitted for the contrast device, the contrast device compares this numerical value and the ratio value of setting for and reachs the contrast signal, the contrast signal that will reachd sends first controller again, the contrast signal control second controller operation that first controller sent according to the contrast device when controlling the operation of first governing valve, and the flow of second governing valve is adjusted according to the contrast signal that first controller sent and according to the ratio value of setting for to the second controller, can effectively reduce the influence of error like this, improve the ratio precision between each reaction material, the inaccurate problem of ratio when effectively preventing to add reaction material.
Drawings
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is a control flow diagram of the present invention.
The reference numbers in the figures are: 100. a kettle body; 110. a kettle cover; 200. a stirring device; 210. a stirring shaft; 220. a drive motor; 230. a stirring blade; 240. parallel blades; 300. a first storage tank; 310. a first feed tube; 320. a first feed tube; 330. a first pump; 340. a first liquid level sensing device; 400. a second storage tank; 410. a second feed tube; 420. a second feed tube; 430. a second pump; 440. a second liquid level sensing device; 500. a control device; 510. a first controller; 520. a first regulating valve; 530. a second controller; 540. a second regulating valve; 550. a third regulating valve; 560. a fourth regulating valve; 600. an adjustment device; 610. a flow meter; 620. and (5) a comparison device.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some, but not all, embodiments of the present application. All other embodiments that can be derived by one of ordinary skill in the art from the embodiments given herein are intended to be within the scope of the present disclosure.
The terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It will be appreciated that the data so used may be interchanged under appropriate circumstances such that embodiments of the application may be practiced in sequences other than those illustrated or described herein, and that the terms "first," "second," and the like are generally used herein in a generic sense and do not limit the number of terms, e.g., the first term can be one or more than one. In addition, "and/or" in the specification and claims means at least one of connected objects, a character "/" generally means that a preceding and succeeding related objects are in an "or" relationship.
The following describes in detail the method and apparatus for preparing electronic-grade hexamethyldisilazane, according to the embodiments of the present application, with reference to the accompanying drawings.
Example 1:
the embodiment of the application provides a preparation method of electronic-grade hexamethyldisilazane, which comprises the following steps: the method comprises the following steps:
s1, preparing materials, namely preparing certain amounts of trimethylchlorosilane, carbonate, hexamethyldisiloxane and sulfuric acid, wherein the weight part ratio of the trimethylchlorosilane to the carbonate to the hexamethyldisiloxane is 100: 50-90: 30-180; s2: the preliminary reaction, adding the measured carbonate and hexamethyldisiloxane into a reaction kettle, stirring, adding trimethylchlorosilane into the reaction kettle for reaction, cooling the mixed liquid after the reaction is stopped, and obtaining high-purity hexamethyldisiloxane through centrifugal separation after cooling; s3: comprehensive reaction, namely mixing and reacting metered hexamethyldisiloxane and sulfuric acid, and removing the sulfuric acid by a standing method after the reaction to obtain silicone grease; s4: and (3) preparing a finished product, adding the silicone grease into the pressure kettle, adding benzene, dissolving and stirring, continuously introducing ammonia gas during stirring to react to generate hexamethyldisilazane and ammonium salt, and centrifuging to remove the ammonium salt to obtain the hexamethyldisilazane.
In addition, the mole ratio of hexamethyldisiloxane to inorganic acid is 1: 0.6-0.85 or 1: 4-18.
Further, in S2, trimethylchlorosilane is added dropwise to the mixture of carbonate, hexamethyldisiloxane and the mixture.
Example 2:
the embodiment of the application provides production equipment of electronic-grade hexamethyldisilazane, and in addition to the technical characteristics, the production equipment of electronic-grade hexamethyldisilazane further comprises the following technical characteristics.
As shown in fig. 1, including reation kettle, reation kettle includes the cauldron body 100, sets up kettle cover 110 on the cauldron body 100 and sets up agitating unit 200 in the cauldron body 100, and reation kettle still includes feeding device, and feeding device includes: the first storage tank 300 is used for storing materials for reaction, a first feeding pipe 310 is arranged between the first storage tank 300 and the reaction kettle, a first feeding pipe 320 is further arranged on the first storage tank 300, and a first pump 330 is further arranged on the first feeding pipe 310; a second storage tank 400 for storing reaction materials, a second feeding pipe 410 arranged between the second storage tank 400 and the reaction kettle, a second feeding pipe 420 arranged on the second storage tank 400, and a second pump 430 arranged on the second feeding pipe 410; the reaction device further comprises a control device 500, the control device 500 is connected with the first pump 330 and the second pump 430 and controls the first pump 330 and the second pump 430, and the control device 500 can input a ratio value required by the reaction so as to control the first pump 330 and the second pump 430 to deliver reaction materials with corresponding values according to the input ratio value.
In this embodiment of the application, through being equipped with controlling means 500, can control first pump 330 and second pump 430, when needs react, the staff will need the ratio value between the material of reaction to input controlling means 500, controlling means 500 can be through the required ratio value of input reaction thereby control first pump 330 and second pump 430 carry the material for the reaction of corresponding numerical value according to the ratio value of input, first bin 300 and second bin 400 are used for storing the material for reaction, the bin can increase according to the promotion of the material kind that needs the reaction, control can be to the automatic reaction material that adds in reation kettle through being equipped with controlling means 500, needn't artifical the interpolation, and whole process is gone on under encapsulated situation, can improve the quality and the efficiency of reaction, and simultaneously, can also improve the accuracy of reaction.
Furthermore, the control device 500 includes: a first controller 510, wherein the first controller 510 comprises a first regulating valve 520 connected with the first pump 330, and the first regulating valve 520 is arranged on the first feeding pipe 310; a second controller 530, wherein the second controller 530 comprises a second regulating valve 540 connected to the second pump 430, and the second regulating valve 540 is disposed on the second feeding pipe 410; the first controller 510 controls the first regulating valve 520 to operate, the first controller 510 is connected with the second controller 530 and controls the second controller 530 to operate, the first controller 510 controls the first regulating valve 520 to operate according to a set proportioning value, meanwhile, the first controller 510 controls the second controller 530 to operate, and the second controller 530 controls the second regulating valve 540 to operate according to a command sent by the first controller 510 and according to the set proportioning value.
In some embodiments of the present application, the first controller 510 may control the operation of the second controller 530 while controlling the operation of the first regulating valve 520, and the second controller 530 may control the operation of the second regulating valve 540 according to a command sent by the first controller 510 and according to a set proportioning value, and the above operation manner is adopted to implement real-time detection and correction on the process of conveying different reaction materials by the first pump 330 and the second pump 430, so as to ensure the accuracy of the ratio between different materials to react according to the proportioning value input by the user strictly and the qualification rate.
Example 3:
the embodiment of the application provides production equipment of electronic-grade hexamethyldisilazane, and in addition to the technical characteristics, the production equipment of electronic-grade hexamethyldisilazane further comprises the following technical characteristics.
As shown in fig. 1 and 2, the control device 500 further includes an adjusting device 600, and the adjusting device 600 includes: the flow meter 610 is arranged on the first feeding pipe 310 and used for detecting and feeding back the flow of the first pump 330; the comparison device 620 is connected with the flowmeter 610, and the comparison device 620 is used for receiving the flow value fed back by the flowmeter 610, comparing the flow value with a set proportioning value to obtain a comparison signal, and sending the obtained comparison signal to the first controller 510; the first controller 510 controls the operation of the first adjusting valve 520 and simultaneously controls the operation of the second controller 530 according to the comparison signal sent by the comparison device 620, and the second controller 530 adjusts the flow rate of the second adjusting valve 540 according to the comparison signal sent by the first controller 510 and according to the set ratio.
In the embodiment of the present application, the adjusting device 600 is provided to enable the control of the first adjusting valve 520 and the second adjusting valve 540 to be more precise, when the adjustment is performed, the flow meter 610 detects the flow rate of the first pump 330, that is, the first storage tank 300 inputs a value reflecting the material into the reaction kettle, the detected value is transmitted to the comparison device 620, the comparison device 620 compares the value with a set proportioning value to obtain a comparison signal, and then transmits the obtained comparison signal to the first controller 510, the first controller 510 controls the operation of the first adjusting valve 520 and simultaneously controls the operation of the second controller 530 according to the comparison signal transmitted by the comparison device 620, and the second controller 530 adjusts the flow rate of the second adjusting valve 540 according to the comparison signal transmitted by the first controller 510 and according to the set proportioning value, so as to effectively reduce the influence of errors and improve the proportioning precision between the reaction materials, effectively preventing the problem of inaccurate ratio when adding reaction materials.
Example 4:
the embodiment of the application provides production equipment of electronic-grade hexamethyldisilazane, and in addition to the technical characteristics, the production equipment of electronic-grade hexamethyldisilazane further comprises the following technical characteristics.
As shown in fig. 1 and 2, a first liquid level sensing device 340 is disposed in the first storage tank 300, a second liquid level sensing device 440 is disposed in the second storage tank 400, a third adjusting valve 550 is further disposed on the first feeding pipe 320, a fourth adjusting valve 560 is disposed on the second feeding pipe 420, and the first liquid level sensing device 340, the second liquid level sensing device 440, the third adjusting valve 550 and the fourth adjusting valve 560 are all connected to the first controller 510.
In the embodiment of the present application, when the first liquid level sensing device 340 detects that the liquid level of the reaction material stored in the first storage tank 300 is lower than the set minimum liquid level, the first controller 510 controls the third regulating valve 550 to open, so as to inject the reaction material from the first feeding pipe 320 into the first storage tank 300 until the liquid level in the first storage tank 300 reaches the set maximum liquid level; when the second liquid level sensing device 440 detects that the liquid level of the reaction material stored in the second storage tank 400 is lower than the set lowest liquid level, the first controller 510 controls the fourth regulating valve 560 to open, so that the reaction material is injected into the second storage tank 400 from the second feeding pipe 420 until the liquid level in the second storage tank 400 reaches the set highest liquid level, the material can be automatically added, the processing time is saved, and the processing efficiency is improved.
Example 5:
the embodiment of the application provides production equipment of electronic-grade hexamethyldisilazane, and in addition to the technical characteristics, the production equipment of electronic-grade hexamethyldisilazane further comprises the following technical characteristics.
As shown in fig. 1, the stirring device 200 includes: a stirring shaft 210; one end of the stirring shaft 210 is provided with a driving motor 220 for driving the stirring shaft 210 to rotate; the stirring blades 230 are spirally arranged on the stirring shaft 210, two stirring blades 230 are symmetrically arranged on the stirring shaft 210, and the spiral directions of the two stirring blades 230 are opposite; wherein, the blade surface of the stirring blade 230 faces the axial direction of the kettle body 100, the two ends of the two stirring blades 230 are both provided with parallel blades 240, and the other ends of the parallel blades 240 are connected with the stirring shaft 210.
Further, set up stirring vane 230 on (mixing) shaft 210 with screw means, when preventing that the material in the reaction cauldron stirs, the reaction material forms the material circulation in the outside and the inside of the spiral that helical blade formed, the reaction material that is located the spiral outside flows upwards under helical blade's effect, simultaneously, the material that is located the internal top of cauldron 100 flows downwards after getting into the spiral inside, thereby form the material circulation, the material mixes with higher speed, the material mixing effect homogeneous that makes different positions in the cauldron body 100, product quality has effectively been improved.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. Further, it should be noted that the scope of the methods and apparatus of the embodiments of the present application is not limited to performing the functions in the order illustrated or discussed, but may include performing the functions in a substantially simultaneous manner or in a reverse order based on the functions involved, e.g., the methods described may be performed in an order different than that described, and various steps may be added, omitted, or combined. In addition, features described with reference to certain examples may be combined in other examples.
While the present embodiments have been described with reference to the accompanying drawings, it is to be understood that the invention is not limited to the precise embodiments described above, which are meant to be illustrative and not restrictive, and that various changes may be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A preparation method of electronic-grade hexamethyldisilazane is characterized by comprising the following steps: the method comprises the following steps:
s1, preparing materials, namely preparing certain amounts of trimethylchlorosilane, carbonate, hexamethyldisiloxane and sulfuric acid, wherein the weight part ratio of the trimethylchlorosilane to the carbonate to the hexamethyldisiloxane is 100: 50-90: 30-180;
s2: the preliminary reaction, adding the measured carbonate and hexamethyldisiloxane into a reaction kettle, stirring, adding trimethylchlorosilane into the reaction kettle for reaction, cooling the mixed liquid after the reaction is stopped, and obtaining high-purity hexamethyldisiloxane through centrifugal separation after cooling;
s3: comprehensive reaction, namely mixing and reacting metered hexamethyldisiloxane and sulfuric acid, and removing the sulfuric acid by a standing method after the reaction to obtain silicone grease;
s4: and (3) preparing a finished product, adding the silicone grease into the pressure kettle, adding benzene, dissolving and stirring, continuously introducing ammonia gas during stirring to react to generate hexamethyldisilazane and ammonium salt, and centrifuging to remove the ammonium salt to obtain the hexamethyldisilazane.
2. The method of claim 1, wherein the method comprises: the mole ratio of the hexamethyldisiloxane to the inorganic acid is 1: 0.6-0.85 or 1: 4-18.
3. The method of claim 2, wherein the method comprises: in S2, the trimethylchlorosilane is dropped into the carbonate, the hexamethyldisiloxane, and the mixed solution in a dropping manner.
4. The apparatus of claim 3, wherein the apparatus comprises: including reation kettle, reation kettle include the cauldron body (100), set up in kettle cover (110) on the cauldron body (100) and set up in agitating unit (200) in the cauldron body (100), reation kettle still includes feeding device, feeding device includes:
the reaction kettle is characterized by comprising a first storage tank (300) for storing reaction materials, wherein a first feeding pipe (310) is arranged between the first storage tank (300) and the reaction kettle, a first feeding pipe (320) is further arranged on the first storage tank (300), and a first pump (330) is further arranged on the first feeding pipe (310);
the second storage tank (400) is used for storing reaction materials, a second feeding pipe (410) is arranged between the second storage tank (400) and the reaction kettle, a second feeding pipe (420) is further arranged on the second storage tank (400), and a second pump (430) is further arranged on the second feeding pipe (410);
the reaction device further comprises a control device (500), the control device (500) is connected with the first pump (330) and the second pump (430) and controls the first pump (330) and the second pump (430), and the control device (500) can control the first pump (330) and the second pump (430) to convey the reaction materials with corresponding values according to the input proportioning values by inputting the proportioning values required by the reaction.
5. The apparatus of claim 4, wherein the apparatus comprises: the control device (500) comprises:
a first controller (510), the first controller (510) comprising a first regulating valve (520) connected to the first pump (330), the first regulating valve (520) being disposed on the first feeding pipe (310);
a second controller (530), wherein the second controller (530) comprises a second regulating valve (540) connected with the second pump (430), and the second regulating valve (540) is arranged on the second feeding pipe (410);
the first controller (510) controls the first regulating valve (520) to operate, the first controller (510) is connected with the second controller (530) and controls the second controller (530) to operate, the first controller (510) controls the first regulating valve (520) to operate according to a set proportioning value, meanwhile, the first controller (510) controls the second controller (530) to operate, and the second controller (530) controls the second regulating valve (540) to operate according to a set proportioning value according to a command sent by the first controller (510).
6. The apparatus of claim 5, wherein the apparatus comprises: the control device (500) further comprises an adjustment device (600), the adjustment device (600) comprising:
the flowmeter (610) is arranged on the first feeding pipe (310) and used for detecting and feeding back the flow of the first pump (330);
the comparison device (620) is connected with the flowmeter (610), and the comparison device (620) is used for receiving the flow value fed back by the flowmeter (610), comparing the flow value with a set proportioning value to obtain a comparison signal, and sending the obtained comparison signal to the first controller (510);
the first controller (510) controls the operation of the first regulating valve (520) and simultaneously controls the operation of the second controller (530) according to the comparison signal sent by the comparison device (620), and the second controller (530) regulates the flow of the second regulating valve (540) according to the comparison signal sent to the first controller (510) and the set ratio value.
7. The apparatus of claim 6, wherein the apparatus comprises: be equipped with first liquid level induction system (340) in first bin (300), be equipped with second liquid level induction system (440) in second bin (400), still be equipped with third governing valve (550) on first inlet pipe (320), can be equipped with fourth governing valve (560) on second inlet pipe (420), just first liquid level induction system (340), second liquid level induction system (440), third governing valve (550) and fourth governing valve (560) all are connected with first controller (510).
8. The apparatus of claim 7, wherein the apparatus comprises: the stirring device (200) comprises:
a stirring shaft (210); one end of the stirring shaft (210) is provided with a driving motor (220) for driving the stirring shaft (210) to rotate;
the stirring blades (230) are spirally arranged on the stirring shaft (210), two stirring blades (230) are symmetrically arranged on the stirring shaft (210), and the spiral directions of the two stirring blades (230) are opposite;
wherein, the blade surface orientation of stirring vane (230) the axis direction of the cauldron body (100), the both ends of two stirring vane (230) all are equipped with parallel blade (240), the other end of parallel blade (240) with (mixing) shaft (210) are connected.
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