CN113583035B - Method for preparing bis (3-trimethoxysilylpropyl) ethylenediamine by using microchannel reactor - Google Patents
Method for preparing bis (3-trimethoxysilylpropyl) ethylenediamine by using microchannel reactor Download PDFInfo
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- HZGIOLNCNORPKR-UHFFFAOYSA-N n,n'-bis(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCNCCC[Si](OC)(OC)OC HZGIOLNCNORPKR-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 14
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- OXYZDRAJMHGSMW-UHFFFAOYSA-N 3-chloropropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCCl OXYZDRAJMHGSMW-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000004821 distillation Methods 0.000 claims abstract description 5
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-Diisopropylethylamine (DIPEA) Chemical compound CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 8
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 abstract description 4
- 238000005580 one pot reaction Methods 0.000 abstract description 2
- 229920001296 polysiloxane Polymers 0.000 abstract 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 abstract 2
- 239000000243 solution Substances 0.000 abstract 1
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 11
- 238000003860 storage Methods 0.000 description 10
- 239000000047 product Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- -1 3-trimethoxysilylpropyl Chemical group 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- BYIMSFXYUSZVLI-UHFFFAOYSA-N 3-methoxysilylpropan-1-amine Chemical compound CO[SiH2]CCCN BYIMSFXYUSZVLI-UHFFFAOYSA-N 0.000 description 1
- TZZGHGKTHXIOMN-UHFFFAOYSA-N 3-trimethoxysilyl-n-(3-trimethoxysilylpropyl)propan-1-amine Chemical compound CO[Si](OC)(OC)CCCNCCC[Si](OC)(OC)OC TZZGHGKTHXIOMN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
-
- 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
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a method for preparing bis (3-trimethoxy-silicone propyl) ethylenediamine by a microchannel reactor, which comprises the steps of taking 3-chloropropyl-trimethoxy silane as a raw material, mixing ethylenediamine, an acid binding agent and ethanol serving as a solvent to obtain an ethylenediamine mixed solution, respectively pumping the ethylenediamine mixed solution and the 3-chloropropyl-trimethoxy-silane into a direct-current microchannel for preheating and mixing to form a reaction material, enabling the preheated and mixed reaction material to enter an enhanced mass transfer microchannel for reaction, enabling the obtained solution to flow out from an outlet of the enhanced mass transfer microchannel after the reaction, and carrying out reduced pressure distillation to obtain the bis (3-trimethoxy-silicone propyl) ethylenediamine. The invention utilizes a microchannel reactor to directly generate the bis (3-trimethoxysilylpropyl) -ethylenediamine by the one-step reaction of the 3-chloropropyltrimethoxysilane and ethylenediamine under the conditions of high temperature and high pressure, thereby solving the problems of long reaction time and low yield in the prior art.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for preparing an aminosilane coupling agent-bis (3-trimethoxysilylpropyl) ethylenediamine by adopting a microchannel reactor.
Background
Bis (3-trimethoxysilylpropyl) ethylenediamine, also known as: n, N' -bis (3-trimethoxysilylpropyl) ethyl-1, 2-diamine is an important industrial additive, has a structural formula shown in the specification, and is widely used for modifying coupling agents, coatings and fireproof materials.
In patent WO 2019/093259 Al a process for the synthesis of bis (3-trimethoxysilylpropyl) ethylenediamine by reaction of N- (2-aminoethyl) -3-aminopropyl trimethoxysilane with 3-chloropropyl trimethoxysilane is mentioned, but specific process parameters and final yields are not involved. Wherein the N- (2-aminoethyl) -3-aminopropyl trimethoxysilane can be synthesized from 3-chloropropyl trimethoxysilane and ethylenediamine.
Patent CN102300869a mentions a pot synthesis method of bis (silylorgano) amine, which synthesizes bis (silylorgano) amine by using halogenated organosilane and amino organosilane as raw materials. The patent mentions that bis (3-trimethoxysilylpropyl) ethylenediamine can be synthesized in a yield of at least 85%. The patent states that: 3-chloropropyl trimethoxy silane and 3-aminopropyl methoxy silane are used as raw materials to react at 130 ℃, ethylenediamine is added midway to assist in layering of reaction liquid (ethylenediamine plays a role of acid binding agent), the lower layer is removed after layering, and the upper layer is distilled under reduced pressure to obtain bis (3-trimethoxy silylpropyl) amine. The reaction is carried out in an autoclave for 4 hours, the final yield is only 81%, and the additional operation (adding ethylenediamine) is needed in the middle, so that continuous production is not realized, and the amino organosilane used as the raw material has no advantage in terms of cost.
Disclosure of Invention
The invention aims to provide a process for synthesizing bis (3-trimethoxysilylpropyl) ethylenediamine by a microchannel reactor, which can realize continuous and stable production and increase production efficiency.
In order to solve the technical problems, the invention provides a method for preparing bis (3-trimethoxysilylpropyl) ethylenediamine by a microchannel reactor, which takes 3-chloropropyl trimethoxysilane as a raw material and comprises the following steps:
firstly, ethylenediamine and an acid binding agent are mixed according to the proportion of 1: 2-2.5, and then adding ethanol serving as a solvent to obtain an ethylenediamine mixed solution, wherein the volume concentration of ethylenediamine in the ethylenediamine mixed solution is 8-12% (preferably 10%);
pumping the ethylenediamine mixed solution and 3-chloropropyl trimethoxysilane into a direct-current micro-channel respectively for preheating and mixing to form a reaction material, and controlling ethylenediamine: 3-chloropropyl trimethoxysilane=1:2-2.2 molar ratio; the temperature of the direct-flow type micro-channel is 100-160 ℃, the preheated and mixed reaction materials enter the enhanced mass transfer type micro-channel, the reaction is carried out under the pressure of 2-4 MPa and the temperature of 100-160 ℃, and the residence time of the reaction materials in the enhanced mass transfer type micro-channel is 30-50 min;
and (3) carrying out reduced pressure distillation on the obtained liquid after the reaction, and flowing out from the outlet of the enhanced mass transfer type micro-channel to obtain the bis (3-trimethoxysilylpropyl) ethylenediamine.
Description: the pressure is regulated by a back pressure valve, preheat temperature in the straight flow microchannel = reaction temperature in the enhanced mass transfer microchannel. The reaction mass was preheated in the straight-flow microchannel for a mixing time (residence time) of about 5 to 10 minutes.
Improvement of the process for preparing bis (3-trimethoxysilylpropyl) ethylenediamine as a microchannel reactor of the present invention:
the acid binding agent is pyridine, triethylamine, diisopropylethylamine (preferably) or triethanolamine.
Further improvement of the process for preparing bis (3-trimethoxysilylpropyl) ethylenediamine as a microchannel reactor of the present invention:
the reaction temperature in the enhanced mass transfer type micro-channel is 140-150 ℃, and the reaction pressure is 3.5-4 Mpa;
controlling ethylenediamine: 3-chloropropyl trimethoxysilane = 1:2 molar ratio;
the residence time of the reaction materials in the enhanced mass transfer type micro-channel is 40-50 min.
The invention has the following technical advantages:
1. the raw materials adopted by the invention are low-cost and easily available ethylenediamine, so that the production cost can be reduced;
2. the invention greatly shortens the reaction time and has high selectivity;
3. the invention has convenient operation, no stop in the reaction midway, and is convenient for realizing automatic control;
4. the invention adopts the micro-channel reactor, has good repeatability, stable product quality and no amplification effect, and can adjust the productivity according to actual needs.
In summary, the invention utilizes a microchannel reactor to directly generate the bis (3-trimethoxysilylpropyl) -ethylenediamine by the one-step reaction of the 3-chloropropyl trimethoxysilane and ethylenediamine under the conditions of high temperature and high pressure, thereby solving the problems of long reaction time and low yield.
Drawings
The following describes the embodiments of the present invention in further detail with reference to the accompanying drawings.
FIG. 1 is a schematic representation of a reactor apparatus for use in the present invention.
Detailed Description
The following describes embodiments of the present invention in detail: the present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are provided, but the protection scope of the present invention is not limited to the following embodiments.
An example of the device, a microchannel reaction device, comprises a storage tank 1 for storing ethylenediamine mixed solution, and a storage tank 3 for storing 3-chloropropyl trimethoxysilane;
the storage tank 1 is connected with the inlet of the direct-current type micro-channel 5 after passing through the feed pump 2, the storage tank 3 is connected with the inlet of the direct-current type micro-channel 5 after passing through the feed pump 4, the outlet of the direct-current type micro-channel 5 is connected with the inlet of the enhanced mass transfer type micro-channel 6, the outlet of the enhanced mass transfer type micro-channel 6 is provided with a back pressure valve 7, and the outlet of the enhanced mass transfer type micro-channel 6 is connected with the inlet of the receiving tank 8 after passing through the back pressure valve 7.
A valve 11 is arranged on a pipeline between the storage tank 1 and the feed pump 2, a valve 12 is arranged on a pipeline between the feed pump 2 and the direct-current type micro-channel 5, a valve 13 is arranged on a pipeline between the storage tank 3 and the feed pump 4, a valve 14 is arranged on a pipeline between the feed pump 4 and the direct-current type micro-channel 5, and a valve 15 is arranged on a pipeline between the back pressure valve 7 and an inlet of the receiving tank 8. A conventional safety valve 16 is provided on the receiving tank 8. When the pressure in the receiving tank 8 exceeds the set value of the relief valve 16, the relief valve 16 is tripped to release the pressure. The bottom of the receiving tank 8 is provided with a conventional outlet valve.
In actual use, the ethylenediamine mixed solution in the storage tank 1 is conveyed to the direct-current type micro-channel 5 through the feed pump 2, and the 3-chloropropyl trimethoxysilane in the storage tank 3 is conveyed to the direct-current type micro-channel 5, and flows back into the mass transfer enhancement micro-channel 6 for reaction after being fully preheated and mixed. The obtained reaction liquid flows into a receiving tank 8 and is collected, and finally, the product of bis (3-trimethoxysilylpropyl) ethylenediamine is obtained through conventional reduced pressure distillation and purification.
At the beginning, the flow rates of the metering pump 2 and the metering pump 4 are set, the temperatures of the direct-flow type micro-channel 5 and the mass transfer enhancement type micro-channel 6 are set, after the temperatures reach the set temperatures, the valve 11 and the valve 13 are opened, the metering pump 2 and the metering pump 4 are started, and then the back pressure valve 7, the valve 12, the valve 14 and the valve 15 are rapidly opened.
After the reaction is completed, the bottom outlet valve of the receiving tank 8 is opened, and the reaction liquid of the receiving tank 8 is discharged and then subjected to subsequent reduced pressure distillation to separate out the product.
Description: during the feeding of the feed pump 2, 4, the bottom outlet valve of the collection tank 8 is always closed. Therefore, the volume of the collection tank 8 is required to ensure that the reaction product liquid is contained.
The storage tank 1, the storage tank 3 and the receiving tank 8 are respectively provided with a liquid level meter, and the liquid level meter is used for measuring the volume of the corresponding materials in the tank.
In the following cases, the liquid holdup of the direct flow type microchannel 5 is about 12mL, the total liquid holdup of the enhanced mass transfer type microchannel 6 is about 60mL, and the pipe diameter is, for example, 50 to 100. Mu.m.
The following examples were prepared using the device examples described above.
Example 1-1, a method for preparing bis (3-trimethoxysilylpropyl) ethylenediamine, comprising the steps of:
1) Firstly, ethylenediamine and diisopropylethylamine as an acid binding agent are mixed according to a volume ratio of 1:2, mixing, and adding ethanol serving as a solvent to prepare an ethylenediamine mixed solution, wherein the volume concentration of ethylenediamine in the mixed solution is 10%;
3-chloropropyl trimethoxysilane is used as a raw material for standby;
2) Pumping the ethylenediamine mixed solution and 3-chloropropyl trimethoxysilane into a direct-current micro-channel 5 through a feed pump 2 and a feed pump 4 respectively to preheat and mix to form a reaction material, and controlling the flow rate to control ethylenediamine: 3-chloropropyl trimethoxysilane = 1:2 molar ratio; the temperature in the direct-current type micro-channel 5 is 140 ℃, and the residence time of the reaction materials in the direct-current type micro-channel 5 is about 8min;
the preheated reaction material enters the enhanced mass transfer type micro-channel 6, the reaction temperature in the enhanced mass transfer type micro-channel 6 is controlled to 140 ℃, and the back pressure valve 7 is controlled to enable the preheated reaction material to react in the enhanced mass transfer type micro-channel 6 under the pressure of 3.5MPa, wherein the reaction time (the residence time of the preheated reaction material in the enhanced mass transfer type micro-channel 6) is 40min.
3) The liquid obtained after the reaction flowing out from the outlet of the enhanced mass transfer type micro-channel 6 is collected by a collecting tank 8, discharged through an outlet valve at the bottom of the collecting tank 8, distilled under the pressure of-97 KPa and collected at the temperature of 240-260 ℃ to obtain the bis (3-trimethoxysilylpropyl) ethylenediamine.
Examples 1-2 to 1-8,
The temperatures of the direct flow type microchannel 5 and the enhanced mass transfer type microchannel 6 were changed, and the rest was the same as in example 1-1. The product yield was checked to give the following data (Table 1).
TABLE 1 influence of reaction temperature on yield
Examples 2-1 to 2-3
With respect to example 1-1, only the kind of the acid-binding agent was changed (molar amount was kept unchanged), and the rest was equivalent to example 1-1. The product yield was checked to give the following data (Table 2).
TABLE 2 influence of acid binding agent on yield
Examples 3-1 to 3-4
With respect to example 1-1, ethylenediamine: the molar ratio of 3-chloropropyl trimethoxysilane was kept unchanged, and the residence time of the reaction mass in the enhanced mass transfer microchannel 6 was changed by changing the flow rates of the feed pump 2 and the feed pump 4, etc., the remainder being equivalent to example 1-1. The product yield was checked to give the following data (Table 3).
TABLE 3 influence of reaction residence time on yield
Examples 4-1 to 4-2
In contrast to example 1-1, ethylenediamine was adjusted: the feed molar ratio of 3-chloropropyl trimethoxysilane, the residence time of the reaction mass in the enhanced mass transfer microchannel 6 remains unchanged, the remainder being identical to example 1-1. The product yield was checked to give the following data (Table 4).
TABLE 4 influence of flow rate on yield
Examples 5-1 to 5-5
The reactor pressure was varied by adjusting the back pressure valve 7 in comparison to example 1-1, the remainder being identical to example 1-1. The product yield was checked to give the following data (Table 5).
TABLE 5 influence of reactor pressure on yield
EXAMPLE 6,
With respect to example 1-1, ethylenediamine: the volume ratio of diisopropylethylamine is defined by "1:2 "1:2.5", the volume concentration of ethylenediamine in the ethylenediamine mixed solution was unchanged, still 10%, the remainder was identical to example 1-1, and the final yield was 86.0%.
Comparative example 1,
Comparative example 1 was changed from ethanol to methanol with respect to example 1-1, and the rest was identical to example 1-1, resulting in a final yield of 84.9%. This case is not as environmentally friendly as the present invention.
Comparative example 2-1
In contrast to example 1-1, comparative example 2 did not add an acid-binding agent, and the ethylenediamine mixed solution did not contain diisopropylethylamine as an acid-binding agent, i.e., ethylenediamine and ethanol were formulated into an ethylenediamine mixed solution having an ethylenediamine volume concentration of 10%; the remainder was identical to example 1-1, with a final yield of 41.9%.
Comparative examples 2 to 2
With respect to example 1-1, ethylenediamine: the volume ratio of diisopropylethylamine is defined by "1:2 "1:1.5", the volume concentration of ethylenediamine in the ethylenediamine mixed solution was unchanged, still 10%, the remainder was identical to example 1-1, and the final yield was 80.3%.
Comparative examples 3-1 to 3-3
Comparative examples 3-1 to 3-3 were obtained by changing the reactor pressure by adjusting the back pressure valve in comparison with example 1-1, and the remaining conditions were the same as those of example 1, giving the following data (Table 6)
TABLE 6 final yields for comparative examples 3-1-3
Comparative examples 4-1 to 4-2
In comparative examples 4-1 to 4-2, ethylene diamine, in contrast to example 1-1: the molar ratio of 3-chloropropyl trimethoxysilane was kept constant and the residence time of the reaction mass in the enhanced mass transfer microchannel 6 was varied by varying the flow rates of feed pump 2 and feed pump 4, the remainder being identical to example 1-1. The following data (Table 7) were obtained
TABLE 7 final yields for comparative examples 4-1-4-2
Finally, it should also be noted that the above list is merely a few specific embodiments of the present invention. Obviously, the invention is not limited to the above embodiments, but many variations are possible. All modifications directly derived or suggested to one skilled in the art from the present disclosure should be considered as being within the scope of the present invention.
Claims (3)
1. The method for preparing the bis (3-trimethoxysilylpropyl) ethylenediamine by using the microchannel reactor takes 3-chloropropyl trimethoxysilane as a raw material and is characterized by comprising the following steps of:
firstly, ethylenediamine and an acid binding agent are mixed according to the proportion of 1: 2-2.5, and then adding ethanol serving as a solvent to obtain an ethylenediamine mixed solution, wherein the volume concentration of ethylenediamine in the ethylenediamine mixed solution is 8-12%;
pumping the ethylenediamine mixed solution and 3-chloropropyl trimethoxysilane into a direct-current micro-channel respectively for preheating and mixing to form a reaction material, and controlling ethylenediamine: 3-chloropropyl trimethoxysilane=1:2-2.2 molar ratio; the temperature of the direct flow type micro-channel is 140-160 ℃, the preheated and mixed reaction materials enter the enhanced mass transfer type micro-channel and react under the pressure of 3.5-4 Mpa and the temperature of 140-160 ℃, and the residence time of the reaction materials in the enhanced mass transfer type micro-channel is 30-50 min;
the acid binding agent is pyridine, triethylamine, diisopropylethylamine and triethanolamine;
and (3) carrying out reduced pressure distillation on the obtained liquid after the reaction, and flowing out from the outlet of the enhanced mass transfer type micro-channel to obtain the bis (3-trimethoxysilylpropyl) ethylenediamine.
2. The method for preparing bis (3-trimethoxysilylpropyl) ethylenediamine by using the microchannel reactor according to claim 1, wherein the method comprises the following steps:
controlling ethylenediamine: 3-chloropropyl trimethoxysilane=1:2 molar ratio.
3. The method for preparing bis (3-trimethoxysilylpropyl) ethylenediamine by using the microchannel reactor according to claim 1 or 2, wherein: the residence time is 45 min-50 min.
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| 微化工技术;陈光文等;化工学报;第54卷(第4期);第427-439页 * |
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