CN213596189U - Reaction device for preparing 3-isocyanate propyl trimethoxy silane by continuous method - Google Patents
Reaction device for preparing 3-isocyanate propyl trimethoxy silane by continuous method Download PDFInfo
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- CN213596189U CN213596189U CN202021482759.5U CN202021482759U CN213596189U CN 213596189 U CN213596189 U CN 213596189U CN 202021482759 U CN202021482759 U CN 202021482759U CN 213596189 U CN213596189 U CN 213596189U
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Abstract
The utility model provides a reaction unit for preparing 3-isocyanate propyl trimethoxy silane by a continuous method, which comprises: the device comprises a raw material tank, a buffer tank, a tower reactor, a first condenser and a second condenser; the tower reactor comprises an upper section, a lower section and a middle section which are communicated, wherein the upper section is internally provided with a rectification filler, the lower section is internally provided with a catalyst, and the middle section is provided with a feeding port; the output port of the raw material tank and the output port of the buffer tank are communicated to the middle part of the tower reactor, the input port of the buffer tank is communicated with the bottom of the tower reactor, the top of the upper section of the tower reactor is communicated with the first-stage condenser, and the first-stage condenser is communicated with the second-stage condenser. The utility model has the advantages that: the reaction conversion rate and selectivity are high, and the obtained product has light color; the bottom discharge of the reactor basically has no residue generation, the bed charge is subjected to cyclic reaction, the conversion rate of the raw materials can reach 100 percent, the reaction is stable and controllable, no dangerous operation is caused, and particularly, the reaction can be continuously operated.
Description
Technical Field
The utility model relates to the field of chemistry, in particular to a reaction device for preparing 3-isocyanate propyl trimethoxy silane by a thermal cracking continuous method.
Background
The 3-isocyanate propyl trimethoxy silane is a silane coupling agent containing NCO groups, is an excellent glass fiber treating agent, can improve the mechanical strength, electrical property and ageing resistance of a composite material, and is widely applied to polyethylene crosslinking, such as glass fiber surface treatment of glass fiber reinforced plastics of unsaturated resin, polyethylene, polypropylene resin and the like, surface moisture-proof treatment of synthesized special coatings, adhesives and electronic devices, surface treatment of inorganic silicon fillers and the like.
The currently industrialized methods for preparing isocyanatosilanes are mainly the phosgene (triphosgene) method, the isocyanic acid method and the pyrolysis method. Among them, the pyrolysis method has the advantages of high safety, short reaction time and no waste salt, and is industrially well applied.
Therefore, it is necessary to provide a reaction apparatus for preparing 3-isocyanatopropyltrimethoxysilane by a continuous pyrolysis method.
SUMMERY OF THE UTILITY MODEL
Aiming at the background technology, the utility model aims at providing a 3-isocyanate propyl trimethoxy silane production device which can be operated continuously, has fast cracking speed, less residue, low color and luster and reduced production cost.
In order to achieve the above purpose, the utility model provides a technical scheme is:
a reaction device for preparing 3-isocyanatopropyl trimethoxy silane by a continuous method, which comprises: the device comprises a raw material tank, a buffer tank, a tower reactor, a first condenser and a second condenser; the tower reactor comprises an upper section, a lower section and a middle part between the upper section and the lower section, wherein the upper section and the lower section are communicated with each other; an output port of the raw material tank and an output port of the buffer tank are communicated to the middle part of the tower reactor, an input port of the buffer tank is communicated with the bottom of the tower reactor, the top of the upper section of the tower reactor is communicated with the first condenser, and the first condenser is communicated with the second condenser; the raw material tank is used for placing a raw material of 3-trimethoxy silane methyl carbamate, the raw material enters from the middle of the tower reactor and then reaches the lower section of the tower reactor, the bottom of the lower section is used for discharging reaction residual liquid and discharging the reaction residual liquid into the buffer tank, the top of the upper section of the tower reactor is used for discharging 3-isocyanate propyl trimethoxy silane and methanol, the first condenser is used for condensing to obtain the 3-isocyanate propyl trimethoxy silane, and the second condenser is used for condensing to obtain the methanol.
Preferably, a raw material pump and a mass flow controller are connected between the output port of the raw material tank and the middle part of the tower reactor and/or between the output port of the buffer tank and the middle part of the tower reactor, and a raw material pump is connected between the input port of the buffer tank and the bottom of the tower reactor.
Preferably, the operation pressure of the tower reactor is normal pressure or slightly negative pressure: -0.05 to-0.03 MPa.
The operating temperature of a lower section catalyst layer of the tower reactor is 220-260 ℃, and the operating temperature of an upper section rectification layer is 120-150 ℃; the lower section of the reactor adopts heat conducting oil as a heating medium, and the upper section of the reactor adopts steam as a heating medium.
The cooling medium of the first condenser adopts normal-temperature circulating water or hot water: 30-70 ℃; the cooling medium of the second condenser adopts low-temperature brine: -20 to-10 ℃.
The reaction device for preparing 3-isocyanate propyl trimethoxy silane has the following beneficial effects: the reaction conversion rate and selectivity are high, and the obtained product has light color; the bottom discharge of the reactor basically has no residue generation, the bed charge is subjected to cyclic reaction, the conversion rate of the raw materials can reach 100 percent, the reaction is stable and controllable, no dangerous operation is caused, and particularly, the reaction can be continuously operated.
Drawings
Fig. 1 is a schematic view of a connection relationship of a reaction apparatus according to an embodiment of the present invention.
Detailed Description
This example provides a reaction apparatus for preparing 3-isocyanatopropyltrimethoxysilane by a continuous process, as shown in FIG. 1, comprising: the device comprises a raw material tank 1, a buffer tank 2, a tower reactor 6, a first condenser 7 and a second condenser 8, wherein the tower reactor consists of an upper section 61, a lower section 62 and a middle section 63 between the upper section 61 and the lower section 62 which are communicated, a rectification filler is placed in the upper section 61, a catalyst is placed in the lower section 62, a feeding port is formed in the middle section 63, the middle section 63 is communicated with the lower section 62, so that a raw material 3-trimethoxy silane methyl carbamate can enter the lower section 62 from the middle section 63, the middle section 63 is communicated with the upper section 61, and a structure which can be used for gas circulation but can not pass through solids is specifically set, for example: the baffle structure with a plurality of micropores can enable the product steam in the lower section 62 to reach the rectifying layer upwards, and the rectifying packing in the upper section 61 can not fall off.
The output port of the raw material tank 1 and the output port of the buffer tank 2 are both communicated to the middle part 63 of the tower reactor 6, the input port of the buffer tank 2 is communicated with the bottom of the tower reactor 6, namely the bottom of the lower section 62, the upper section 61 of the tower reactor 6 is communicated with the first condenser 7, and the first condenser 7 is communicated with the second condenser 8. The raw material tank 1 is used for placing a raw material 3-trimethoxy silane methyl carbamate, the raw material enters from the middle part 63 of the tower reactor 6 and then reaches the lower section 62 of the tower reactor 6, the bottom of the lower section 62 is used for discharging reaction residual liquid and discharging the reaction residual liquid into the buffer tank 2, the top of the upper section 61 of the tower reactor 6 is used for discharging isocyanate silane products and methanol, the first condenser 7 is used for condensing to obtain products, and the second condenser 8 is used for condensing to obtain methanol.
A raw material pump and a mass flow controller are connected between the output port of the raw material tank 1 and the middle part 63 of the tower reactor 6, and between the output port of the buffer tank 2 and the middle part 63 of the tower reactor 6, in fig. 1, the raw material pump 3 and the mass flow controller 11 are connected in series between the output port of the raw material tank 1 and the middle part 63 of the tower reactor 6, the raw material pump 4 and the mass flow controller 12 are connected between the output port of the buffer tank 2 and the middle part 63 of the tower reactor 6, and another raw material pump 5 is connected between the input port of the buffer tank 2 and the bottom of the tower reactor 6.
The raw material 3-trimethoxy silane methyl carbamate enters a tower reactor with catalyst from the middle part 63 of the tower reactor through a raw material tank 1, the raw material passes through a catalyst bed layer of a lower section 62 to be cracked, product steam upwards passes through a rectifying layer to be refined to obtain a product 3-isocyanate propyl trimethoxy silane and methanol, and the methanol can be removed by utilizing the boiling point difference to obtain a refined product. After the materials are reacted, discharging materials at the top of the tower reactor 6, namely the top of the upper section 61, to be isocyanate silane products and methanol, condensing the products through a first condenser 7, and condensing the methanol through a second condenser 8 to obtain the product; the residual liquid is discharged from the bottom of the tower reactor 6, namely the bottom of the lower section 62, and can be mixed with fresh raw materials and enter the tower reactor 6 again for cracking reaction.
The operation pressure of the tower reactor 6 is normal pressure or micro negative pressure: -0.05 to-0.03 MPa.
The operation temperature of the catalyst layer of the lower section 62 of the tower reactor 6 is 220-260 ℃, and the operation temperature of the rectification layer of the upper section 61 is 120-150 ℃. The heating medium of the lower section 62 of the tower reactor 6 adopts heat conducting oil, and the heating medium of the upper section 61 of the reactor adopts water vapor.
The cooling medium of the first condenser 7 adopts normal-temperature circulating water or hot water: 30-70 ℃; the cooling medium of the second condenser 8 adopts low-temperature saline water at-20 to-10 ℃.
Example 1
Raw materials in a raw material tank 1 enter from the middle part 63 of a tower type reactor by controlling the flow velocity through a raw material pump 3 and a flow controller 11, a supported catalyst with active components of zinc oxide, titanium oxide and a silicon-aluminum molecular sieve as carriers is used, the space velocity of catalyst raw materials is 0.4g/h/g/cat, the reaction temperature is 220 ℃, the rectification temperature is 120 ℃, the operation pressure is normal pressure, the discharge at the bottom of the reactor is residual liquid, product steam upwards passes through a rectification layer to be refined to obtain a product and methanol, the methanol can be removed by utilizing the boiling point difference to obtain the refined product, the product is obtained by condensing through a first condenser, and the methanol is obtained by condensing through a second condenser. And (3) reaction results: the single conversion rate is 92.7 percent, and the product yield is 84.2 percent.
Example 2
This example further verifies the applicability of the reaction apparatus at different operating temperatures, and the operation process and working principle are the same as those of example 1, except that: the reaction temperatures were adjusted to 230 ℃ and 240 ℃ and the other operating conditions were the same as in example 1. And (3) reaction results: when the reaction temperature is 230 ℃, the single conversion rate is 94.3 percent, and the product yield is 85.0 percent; the reaction temperature is 240 ℃, the single conversion rate is 95.1 percent, and the product yield is 82.5 percent. Examples 1 and 2 show that the reaction apparatus has better applicability in the range of the reaction temperature of 220 ℃ and 240 ℃.
Example 3
This example further demonstrates the applicability of the reaction apparatus at different feed space velocities, the same operational procedure and working principle as in example 1, with the difference that: the feeding space velocity is adjusted to be 0.3g/h/g/cat and 0.2g/h/g/cat, and other operation conditions are as follows: the reaction temperature is 230 ℃, the rectification temperature is 120 ℃, and the operation pressure is normal pressure. And (3) reaction results: when the feeding airspeed is 0.3g/h/g/cat, the single conversion rate is 96.7 percent, and the product yield is 86.7 percent; when the feeding space velocity is 0.2g/h/g/cat, the single conversion rate is 97.2 percent, and the product yield is 83.4 percent. Examples 2 and 3 show that the reaction device has better applicability in the range of the feeding airspeed of 0.2-0.4 g/h/g/cat.
Example 4
This example further demonstrates the applicability of the reactor apparatus at different operating pressures, the same operational procedure and working principle as in example 1, with the following differences: the operating pressure is micro negative pressure-0.04 MPa, and other operating conditions are as follows: the feeding space velocity is 0.3g/h/g/cat, the reaction temperature is 230 ℃, and the rectification temperature is 120 ℃. And (3) reaction results: the single conversion rate is 97.5 percent, and the product yield is 87.8 percent. Examples 3 and 4 demonstrate that the reactor apparatus is well adapted to operation in both the normal pressure and micro-negative pressure ranges.
The above description is further detailed description of the provided technical solutions in connection with the preferred embodiments of the present invention, and it should not be considered that the present invention is limited to the above description, and for those skilled in the art of the present invention, simple deductions and replacements made without departing from the concept of the present invention should be considered as belonging to the protection scope of the present invention.
Claims (4)
1. A reaction device for preparing 3-isocyanatopropyl trimethoxy silane by a continuous method is characterized by comprising the following components: the device comprises a raw material tank, a buffer tank, a tower reactor, a first condenser and a second condenser; the tower reactor comprises an upper section, a lower section and a middle part between the upper section and the lower section, wherein the upper section and the lower section are communicated with each other; an output port of the raw material tank and an output port of the buffer tank are communicated to the middle part of the tower reactor, an input port of the buffer tank is communicated with the bottom of the tower reactor, the top of the upper section of the tower reactor is communicated with the first condenser, and the first condenser is communicated with the second condenser; the raw material tank is used for placing a raw material of 3-trimethoxy silane methyl carbamate, the raw material enters from the middle of the tower reactor and then reaches the lower section of the tower reactor, the bottom of the lower section is used for discharging reaction residual liquid and discharging the reaction residual liquid into the buffer tank, the top of the upper section of the tower reactor is used for discharging 3-isocyanate propyl trimethoxy silane and methanol, the first condenser is used for condensing to obtain the 3-isocyanate propyl trimethoxy silane, and the second condenser is used for condensing to obtain the methanol.
2. The reaction device according to claim 1, wherein a raw material pump and a mass flow controller are connected between the output port of the raw material tank and the middle part of the tower reactor, and/or between the output port of the buffer tank and the middle part of the tower reactor, and a raw material pump is connected between the input port of the buffer tank and the bottom part of the tower reactor.
3. The reaction device according to claim 1, wherein the heating medium at the lower section of the tower reactor is heat conducting oil, and the heating medium at the upper section of the tower reactor is water vapor.
4. The reaction device of claim 1, wherein the cooling medium of the first condenser is normal temperature circulating water or hot water, and the water temperature is 30-70 ℃; the cooling medium of the second condenser adopts low-temperature brine, and the temperature range of the brine is-20 to-10 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662319A (en) * | 2020-07-24 | 2020-09-15 | 浙江皇马科技股份有限公司 | Preparation method of low-color 3-isocyanatopropyl trimethoxy silane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662319A (en) * | 2020-07-24 | 2020-09-15 | 浙江皇马科技股份有限公司 | Preparation method of low-color 3-isocyanatopropyl trimethoxy silane |
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