CN115301187A - Method for preparing hexamethyldisilane amine through inverse concentration gradient reaction - Google Patents

Method for preparing hexamethyldisilane amine through inverse concentration gradient reaction Download PDF

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CN115301187A
CN115301187A CN202211053647.1A CN202211053647A CN115301187A CN 115301187 A CN115301187 A CN 115301187A CN 202211053647 A CN202211053647 A CN 202211053647A CN 115301187 A CN115301187 A CN 115301187A
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reaction
reaction kettle
kettle
concentration gradient
ammonia
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张容
高旭勇
余凯
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Sichuan Jiabi New Material Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • B01J19/1862Stationary reactors having moving elements inside placed in series
    • CCHEMISTRY; METALLURGY
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    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/10Compounds having one or more C—Si linkages containing nitrogen having a Si-N linkage

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Abstract

The invention discloses a method for preparing hexamethyldisilane amine by inverse concentration gradient reaction, which belongs to the technical field of chemical production.A trimethylchlorosilane and ammonia gas are used as raw materials, at least two reaction kettles are arranged for carrying out corresponding at least two reactions, and the trimethylchlorosilane and a solvent are introduced into the first reaction kettle from the upper part of the first reaction kettle; introducing the ammonia gas into the last reaction kettle from the bottom of the last reaction kettle, wherein the ammonia gas flows from the upper part of the next reaction kettle to the bottom of the previous reaction kettle in sequence, the reaction materials are transferred from the previous reaction kettle to the next reaction kettle in sequence, and the materials in the last reaction kettle are transferred to the next step for post-treatment; according to the invention, through carrying out multiple reactions in different reaction kettles and enabling ammonia to flow from the reaction kettle behind to the reaction kettle in front, the concentration of the ammonia is sequentially reduced from the rear end to the front end, the reaction of the trimethylchlorosilane and the ammonia is finally more thorough, and the production efficiency is improved by more than one time.

Description

Method for preparing hexamethyldisilazane by inverse concentration gradient reaction
Technical Field
The invention relates to the technical field of chemical production, in particular to a method for preparing hexamethyldisilane amine through inverse concentration gradient reaction.
Background
Hexamethyldisilazane (HMDS), also known as hexamethyldisilazane, is an important organosilicon reagent and has wide applications in the fields of organosilicon and organic synthesis.
The preparation of hexamethyldisilazane, generally adopt solvent method at present, use trimethyl chlorosilane as raw materials, react with ammonia under the condition of inert solvent, get ammonium chloride and hexamethyldisilazane, hexamethyldisiloxane mixed slurry; the ammonium chloride was removed by separation. Hexamethyldisilazane is present in the filtrate, and the filtrate is distilled to obtain hexamethyldisilazane.
The method is carried out by adopting an intermittent single-pot (single reaction kettle) reaction; taking a single-pot ingredient such as a 3000L kettle as an example, the current preparation method comprises the following steps: the batching ratio is 1200L trimethylchlorosilane, 1200L solvent, after sending into reation kettle, it is not more than 50 ℃ to let in ammonia control temperature, this reaction rate is relatively fast, it is rapid to release heat, consequently, it takes longer time to let in ammonia (25 m year/h) operation, generally need 12 hours initial stage reaction time, later stage decrement keeps ammonia pressure gradually, it takes more than 22 hours to accomplish thorough reaction to feed (send batching and lead in ammonia), and need constantly to adjust the technological parameter of temperature, pressure and ammonia gas volume along with the reaction degree change, the operation is complicated, the operation is out of balance easily causes the material to separate the difficulty. That is, the problems with this current approach include: the material mixing ratio requirement is high, the feeding speed is slow, the reaction time is long (the single-kettle reaction time exceeds 22 h), and the reaction is incomplete. Therefore, how to improve the reaction efficiency and the product quality, which is convenient to operate and easy to control the process parameter index is a technical problem to be solved urgently in the field.
Disclosure of Invention
The invention aims to provide a method for preparing hexamethyldisilane amine by inverse concentration gradient reaction, which solves the problems of incomplete reaction, strict requirements on the material preparation ratio and batch operation in the method for preparing hexamethyldisilane amine.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing hexamethyldisilazane by inverse concentration gradient reaction takes trimethylchlorosilane and ammonia gas as raw materials, at least two reaction kettles are arranged for carrying out corresponding at least two times of reactions, and the trimethylchlorosilane and a solvent are introduced into the first reaction kettle from the upper part of the first reaction kettle; and introducing the ammonia gas into the last reaction kettle from the bottom of the last reaction kettle, wherein the ammonia gas flows to the bottom of the previous reaction kettle from the upper part of the next reaction kettle in sequence, the reaction materials are sequentially transferred from the previous reaction kettle to the next reaction kettle, and the materials of the last reaction kettle are transferred to the next step for post-treatment.
As a preferred technical scheme: the number of the reaction kettles is three, and three reactions are carried out.
The reason why the three reactions are preferably carried out is that: (1) Compared with the feeding amount of the two-time reaction, the feeding amount of the three-time reaction can be larger, and the concentration gradient of the reaction material can be better formed; (2) If the reaction is carried out for two times, the material bearing capacity of the two reaction kettles is small, and the reaction time of the reaction materials is shortened, which is not beneficial to complete reaction; (3) Along with the limitation of reaction process parameters, if more reaction kettles are added, the material feeding amount is not obviously increased any more and the equipment investment is overlarge;
that is, when three times of reactions are carried out, the reaction efficiency can be improved without adding too much equipment while ensuring the reaction to be basically thorough.
As a preferable technical scheme: and quantitatively feeding the trimethylchlorosilane and the solvent into a first reaction kettle. The specific realization mode is that a liquid flow regulating valve is arranged on the liquid material feeding pipe.
As a further preferable technical scheme: the volume ratio of the trimethylchlorosilane to the solvent is 1.
1, the ratio is preferably 1, and the slurry is dispersed and is suitable for separation; when the solvent is too little (such as trimethylchlorosilane: solvent = 2), the dispersion of a slurry viscous (pasty) reaction system is limited, the stirring effect is poor, the slurry cannot be conveyed and separated, the production treatment process is prolonged, and the yield is reduced by 50% compared with 1; when the solvent is too high (such as trimethylchlorosilane: solvent = 1) and the solvent recovery in the subsequent process is increased, the solvent treatment capacity and the distillation treatment capacity are increased under the same yield, the yield per unit time is unchanged, but the energy consumption is increased by about 1.3 times compared with 1.
As a preferable technical scheme: the liquid level in each reaction kettle is dynamically adjusted. The concrete realization mode can be that two ends of the material transferring pump of the material pipeline are respectively provided with a liquid flow regulating valve.
As a further preferred technical solution, the dynamic adjustment method is: taking the depth of a reaction kettle as an example, the liquid level of a detection radar is set to be 1.5m, when the liquid level in the reaction kettle is detected to reach 1.5m, the next reaction kettle starts to pump materials, and when the liquid level is pumped to be 1.0m, namely 1.0m away from the radar liquid level, the material pumping is stopped.
The reason for controlling the radar level mentioned above is that: the mother liquor in the reaction kettle is always kept, the insufficient reaction part in the previous step is dispersed, a diffusion reaction system is adopted, a reaction container is required to be provided with enough 0.2MPa gas phase space, the 0.2MPa coefficient position is 1.5m, so that the ammonia gas reversely flows into the upper layer for reaction, and the reaction efficiency of different stop-pumping material positions is as follows:
radar pumping level (m) radar stop pumping level (m) reaction efficiency (%)
1.5 (safety high position of container) 0.2.70
1.5 (safety high position of container) 0.5
1.5 (Container safety high position) 1.0
1.5 (safety high position of container) 1.2 (but at this time, material is frequently pumped) 98
As a preferred technical scheme: the air pressure in each reaction kettle is dynamically adjusted. The specific implementation mode can be that a gas flow regulating valve is arranged on the ammonia gas feeding pipe.
As a further preferred technical solution, the criteria for dynamically adjusting the air pressure are: the air pressure in the first reaction kettle is 0.1-0.2MPa, and the air pressure in the later reaction kettles is increased by 0.08-0.12MPa in sequence.
By respectively arranging the liquid flow regulating valve and the gas flow regulating valve, the amount of the materials can be accurately controlled, the material ratio is more appropriate, and the reaction is more thorough; the material quantity is controlled by the feeding flow regulating valve, the reaction pressure can be controlled by the gas flow regulating valve, and the ammonia pressure (namely the reaction pressure) is automatically regulated to keep the ammonia excess state all the time, so that the reaction is more thorough.
The liquid flow regulating valve and the gas flow regulating valve are preferably electronic valves, so that online control can be realized, flow control is more accurate and intelligent, and manpower is saved.
In addition: all be provided with pressure detection regulator, temperature detection regulator and level detection regulator in every reation kettle, the aforesaid detects the regulator and is the market purchase, all has the effect of monitoring and regulation simultaneously: the pressure detection regulator is used for feedback linkage regulation and pressure control reaction of the ammonia regulating valve; the temperature detection regulator is used for feedback linkage regulation and temperature control reaction of the feed regulating valve; the liquid level detection and adjustment meter is used for reaction material transfer and pumping linkage adjustment.
The meaning of the "inverse concentration gradient" of the present invention is: after the materials are pumped out of each reaction kettle, the materials are diluted, and after the reaction, the concentration of reactants is reduced, namely, the liquid feeding concentration is reduced in sequence, the ammonia content is increased from low to high, two reaction materials are subjected to reverse concentration reduction reaction in three reaction kettles, and two phases can be effectively dispersed to carry out reaction.
Taking the three reaction kettles as an example, compared with the original single reaction kettle system, the amount of the solvent and the reaction materials is doubled, and the reaction gradient promotes the forward progress of incomplete reaction of trimethylchlorosilane in the dispersion system; the concentration of the materials in the reaction kettle after the material pumping is as follows:
secondary reaction kettle and secondary reaction kettle of primary reaction kettle
High, medium and low trimethyl
Low ammonia concentration, medium concentration and high concentration
0.1MPa saturated ammonia 0.2MPa saturated ammonia 0.3MPa
High reaction rate, medium reaction rate and low reaction rate
The term "trimethyl" as used above refers to trimethylchlorosilane.
The conventional batch reaction refers to: the fixed liquid volume in the reation kettle is the basis, through constantly adding ammonia, there is the violent condition of local reaction, for control reaction process parameter has restricted feeding volume (temperature, pressure height), thereby lead to the reaction extension, if do not lengthen time, control process parameter reacts, there is the incomplete risk of reaction (wherein just included initial stage reaction, middle period reaction and later stage reaction), there is the exhaust of ammonia-containing tail gas in addition, the lost material, increase the environmental protection burden, there is the problem that need take out the material and change the material, thereby occupation equipment, increase equipment occupation time more, present single cauldron production total duration is more than 22 hours, so inefficiency.
After the improved device of the invention is adopted: the device is continuous production, the feeding is more balanced (single pot proportion is not comparable, one pot of raw materials is added for a long time to supplement ammonia for reaction), the idle time of the equipment is zero, the reaction system is more balanced, under the gradient concentration, the primary reaction kettle (namely the first kettle) replaces the primary reaction originally adopting the single reaction kettle, the secondary reaction kettle (namely the second kettle) replaces the middle-stage reaction originally adopting the single reaction kettle, the secondary reaction kettle (namely the third kettle) replaces the later-stage reaction originally adopting the single reaction kettle, the bearing system is enlarged, the dispersion degree of the reaction system is high, no ammonia-containing tail gas is discharged, the process is preferably subjected to bidirectional automatic regulation and control of temperature and pressure, the process is easier to automatically control, the reaction efficiency is more than that of the original single reaction kettle, and the single equipment is improved by more than one time (the yield of the single kettle is about 4 hours and one kettle).
Compared with the prior art, the invention has the advantages that: according to the invention, the plurality of reaction kettles are arranged, and the ammonia flows from the reaction kettle behind to the reaction kettle in front, so that the concentration of the ammonia is sequentially decreased progressively from the rear end to the front end, the concentration inverse gradient of the ammonia is realized, the trimethylchlorosilane and the ammonia are reacted more thoroughly, and the production efficiency is improved by more than one time.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus in embodiment 1 of the present invention.
In the figure: 1. a primary reaction kettle; 2. a secondary reaction kettle; 3. then the reaction kettle is reacted; 4. a first transfer pump; 5. a second material transferring pump; 6. a third material transferring pump; 7. a trimethylchlorosilane feed pipe; 8. an inert solvent feed pipe; 9. a re-reaction ammonia gas feeding pipe; 10. a secondary reaction ammonia gas feeding pipe; 11. an ammonia gas feed pipe for initial reaction.
Detailed Description
The invention will be further explained with reference to the drawings.
Example 1:
first, the present embodiment discloses a device for preparing hexamethyldisilane amine by inverse gradient concentration reaction, the structure of which is shown in fig. 1, comprising three reaction kettles, namely a primary reaction kettle 1, a secondary reaction kettle 2 and a secondary reaction kettle 3,
the upper parts of two adjacent reaction kettles are connected through a material pipeline, a first material transferring pump 4 is arranged on the material pipelines of the primary reaction kettle 1 and the secondary reaction kettle 2 and used for transferring the reacted materials of the primary reaction kettle 1 to the secondary reaction kettle 2, a second material transferring pump 5 is arranged on the material pipelines of the secondary reaction kettle 2 and the secondary reaction kettle 3 and used for transferring the reacted materials of the secondary reaction kettle 2 to the secondary reaction kettle 3, and a third material transferring pump 6 is arranged on the discharge pipeline of the secondary reaction kettle 3 and used for transferring the reacted materials in the secondary reaction kettle 3 to the next working procedure;
the upper end of the primary reaction kettle 1 is connected with a liquid material feeding pipe, the front end of the liquid material feeding pipe is respectively connected with a trimethylchlorosilane feeding pipe 7 and an inert solvent feeding pipe 8, and materials in the trimethylchlorosilane feeding pipe 7 and the inert solvent feeding pipe 8 are gathered in the liquid material feeding pipe;
a secondary reaction ammonia gas inlet pipe 9 is arranged at the bottom of the secondary reaction kettle 3, the secondary reaction ammonia gas inlet pipe 9 is connected with an ammonia gas source, the bottom of the secondary reaction kettle 2 is connected with the upper part of the secondary reaction kettle 3 through a secondary reaction ammonia gas inlet pipe 10, and the bottom of the primary reaction kettle 1 is connected with the upper part of the secondary reaction kettle 2 through a primary reaction ammonia gas inlet pipe 11;
in this embodiment, a liquid flow regulating valve is arranged on the liquid material feeding pipe, liquid flow regulating valves are respectively arranged on the trimethylchlorosilane feeding pipe 7 and the inert solvent feeding pipe 8, liquid flow regulating valves are respectively arranged at two ends of each material transferring pump of the material pipeline, a gas flow regulating valve is arranged on each ammonia gas feeding pipe, and the liquid flow regulating valves and the gas flow regulating valves both adopt electronic valves;
a pressure detection regulator, a temperature detection regulator and a liquid level detection regulator are arranged in each reaction kettle;
a stirring device is arranged in each reaction kettle;
the method for preparing hexamethyldisilane amine by inverse gradient concentration reaction by adopting the device and the principle are as follows:
firstly opening a gas flow valve of a re-reaction ammonia gas feeding pipe 9, introducing ammonia gas into a system, opening gas flow valves of a secondary reaction ammonia gas feeding pipe 10 and a primary reaction ammonia gas feeding pipe 11, filling the whole device with ammonia gas and keeping the pressure of 0.1-0.2MPa, operating a primary reaction kettle 1, controlling and opening liquid flow regulating valves on a trimethyl chlorosilane feeding pipe 7 and an inert solvent feeding pipe 8, automatically regulating the two valves according to the flow ratio of 1, and then sent to the next working procedure for treatment by the third material transferring pump 6.
The third material transferring pump 6 pumps and feeds materials at the bottom of the re-reaction kettle 3, the surplus ammonia gas of the re-reaction kettle 3 is compressed and sent to the secondary reaction kettle 2 from the top of the re-reaction kettle 3, liquid materials which are not completely reacted all the time are transferred to the next step, the reaction residual gas is subjected to the gradient reaction of the previous step, the materials and the ammonia gas which are completely reacted are not mutually soluble, gas and liquid enter the upper step and the lower step of reaction respectively (for example, the liquid after the reaction of the re-reaction kettle 3 enters the next process for treatment, the gas enters the secondary reaction kettle 2 for reaction, the liquid after the reaction of the secondary reaction kettle 2 enters the re-reaction kettle 3 for reaction, and the gas enters the primary reaction kettle 1 for reaction), so that no tail gas containing ammonia is discharged in the whole process.
Setting parameters: setting reaction pressure 0.1-0.2Mpa by PT-1, performing chain reaction on an ammonia feeding regulating valve at an ammonia feeding pipe 9, keeping constant ammonia tail end (initial reaction) 0.1-0.2Mpa for reaction, setting a feeding flow ratio 1 of a trimethylchlorosilane feeding pipe 7 and an inert solvent feeding pipe 8 by TT-1, automatically interlocking the liquid level with a pumping pump, automatically pumping materials in sequence by three material transfer pumps according to a liquid level monitoring result, and controlling the initial liquid level of pumping materials and stopping pumping materials by LT-1, LT-2 and LT-3 radar liquid levels; when the liquid level LT-1 is 1.5 away from the radar, a third material transferring pump 6 is started in a linkage manner to pump to 1.0 away from the radar LT-3; after the pump is stopped and the valve is closed, the second material transferring pump 5 is started in a chain way to pump materials to a position 1.0 away from the radar LT-2; after the pump is stopped and the valve is closed, the first material transferring pump 4 is started to pump materials to a position from the radar LT-1 to the radar 1.0 (namely, the materials are transferred from back to front to a fixed liquid level in the kettle and then stopped).
Compared with the traditional single reaction kettle, the device and the process have the advantages that the yield is improved by about 103 percent in the same time, namely the production efficiency is improved by more than one time.
Comparative example:
1. compared with the example 1, two reaction kettles are adopted, and the rest are the same as the example 1, so that the yield is improved by about 31 percent in the same time compared with the traditional single reaction kettle;
2. compared with the example 1, four reaction kettles are adopted, and the rest are the same as the example 1, so that compared with the traditional single reaction kettle, the yield is improved by about 85% in the same time;
3. compared with the example 1, five reaction kettles are adopted, and the rest are the same as the example 1, so that compared with the traditional single reaction kettle, the yield is improved by about 49% in the same time;
when the number of the reaction kettles is more than three, the more the reaction kettles are, the less the yield is improved, and the less the production efficiency is improved.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (8)

1. A method for preparing hexamethyldisilane amine by inverse concentration gradient reaction takes trimethyl chlorosilane and ammonia gas as raw materials, and is characterized in that: arranging at least two reaction kettles for corresponding at least two reactions, and introducing the trimethylchlorosilane and the solvent into the first reaction kettle from the upper part of the first reaction kettle; and introducing the ammonia gas into the last reaction kettle from the bottom of the last reaction kettle, wherein the ammonia gas flows from the upper part of the next reaction kettle to the bottom of the previous reaction kettle in sequence, the reaction materials are sequentially transferred from the previous reaction kettle to the next reaction kettle, and the materials of the last reaction kettle are transferred to the next step for post-treatment.
2. The process of claim 1, wherein the reaction is a reverse concentration gradient reaction process for the preparation of hexamethyldisilane amine, comprising: the number of the reaction kettles is three, and three reactions are carried out.
3. The process of claim 1, wherein the reaction is a reverse concentration gradient reaction process for the preparation of hexamethyldisilane amine, comprising: and quantitatively feeding the trimethylchlorosilane and the solvent into a first reaction kettle.
4. The process of claim 3, wherein the reaction is carried out in a reverse concentration gradient to form hexamethyldisilane amine: the volume ratio of the trimethylchlorosilane to the solvent is 1.
5. The method of claim 1, wherein the hexamethyldisilane amine is prepared by a reverse concentration gradient reaction, the reverse concentration gradient reaction comprising: the liquid level in each reaction kettle is dynamically adjusted.
6. The method of claim 5, wherein the dynamic adjustment method comprises: taking the depth of the reaction kettle as 2m as an example, the liquid level of the detection radar is set to be 0.5m, when the liquid level in the reaction kettle is detected to reach 1.5m, the next reaction kettle starts to pump materials, and when the liquid level is pumped to be 1.0m, namely, when the liquid level is 1.0m away from the radar, the material pumping is stopped.
7. The method of claim 1, wherein the hexamethyldisilane amine is prepared by a reverse concentration gradient reaction, the reverse concentration gradient reaction comprising: the air pressure in each reaction kettle is dynamically adjusted.
8. The method of claim 7, wherein the pressure dynamic adjustment criteria are: the air pressure in the first reaction kettle is 0.1-0.2MPa, and the air pressure in the later reaction kettles is increased by 0.08-0.12MPa in sequence.
CN202211053647.1A 2022-08-31 2022-08-31 Method for preparing hexamethyldisilane amine through inverse concentration gradient reaction Pending CN115301187A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102351892A (en) * 2011-10-10 2012-02-15 衢州瑞力杰化工有限公司 Production method for hexamethyldisilazane
CN102424407A (en) * 2011-09-08 2012-04-25 韩扶军 Continuous production device for sodium amide
CN104387415A (en) * 2014-11-25 2015-03-04 浙江硕而博化工有限公司 Method for preparing hexamethyl-disilane amine lithium solution and reaction device thereof
CN105367594A (en) * 2015-10-09 2016-03-02 浙江硕而博化工有限公司 Method for preparing hexamethyl-disilazane with hexamethyldisiloxane as raw material
CN114225880A (en) * 2021-12-07 2022-03-25 熵联节能科技(江苏)有限公司 System and method for continuously and efficiently synthesizing hexamethyldisilazane in multi-tower counter-flow manner
CN114409692A (en) * 2022-01-10 2022-04-29 北京莱瑞森医药科技有限公司 Method for preparing hexamethyldisilane amine

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102424407A (en) * 2011-09-08 2012-04-25 韩扶军 Continuous production device for sodium amide
CN102351892A (en) * 2011-10-10 2012-02-15 衢州瑞力杰化工有限公司 Production method for hexamethyldisilazane
CN104387415A (en) * 2014-11-25 2015-03-04 浙江硕而博化工有限公司 Method for preparing hexamethyl-disilane amine lithium solution and reaction device thereof
CN105367594A (en) * 2015-10-09 2016-03-02 浙江硕而博化工有限公司 Method for preparing hexamethyl-disilazane with hexamethyldisiloxane as raw material
CN114225880A (en) * 2021-12-07 2022-03-25 熵联节能科技(江苏)有限公司 System and method for continuously and efficiently synthesizing hexamethyldisilazane in multi-tower counter-flow manner
CN114409692A (en) * 2022-01-10 2022-04-29 北京莱瑞森医药科技有限公司 Method for preparing hexamethyldisilane amine

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