CN111732604B - Preparation method of 3-trimethoxy silane methyl carbamate - Google Patents
Preparation method of 3-trimethoxy silane methyl carbamate Download PDFInfo
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- GTCAXTIRRLKXRU-UHFFFAOYSA-N methyl carbamate Chemical compound COC(N)=O GTCAXTIRRLKXRU-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 50
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 21
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000012043 crude product Substances 0.000 claims abstract description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 238000012805 post-processing Methods 0.000 claims abstract 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 27
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- 150000007529 inorganic bases Chemical group 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 150000007530 organic bases Chemical class 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 abstract description 13
- 239000000126 substance Substances 0.000 abstract description 9
- 239000002360 explosive Substances 0.000 abstract description 2
- 231100000086 high toxicity Toxicity 0.000 abstract description 2
- 231100000053 low toxicity Toxicity 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- MZRVEZGGRBJDDB-UHFFFAOYSA-N N-Butyllithium Chemical compound [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000543 intermediate Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- OSNIIMCBVLBNGS-UHFFFAOYSA-N 1-(1,3-benzodioxol-5-yl)-2-(dimethylamino)propan-1-one Chemical compound CN(C)C(C)C(=O)C1=CC=C2OCOC2=C1 OSNIIMCBVLBNGS-UHFFFAOYSA-N 0.000 description 1
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 239000002318 adhesion promoter Substances 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- -1 isopropanol alcohol amine Chemical class 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000004588 polyurethane sealant Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 239000002966 varnish Substances 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a preparation method of 3-trimethoxy silane methyl carbamate, which comprises the following steps: s1, a reaction process: sequentially adding raw materials of aminosilane, dimethyl carbonate (DMC) and a catalyst into a reactor, wherein the molar ratio of the aminosilane to the dimethyl carbonate is 2:1-4:1, introducing nitrogen into the reactor to replace and discharge air, heating a reaction system to 90-115 ℃ under the condition of stirring, and reacting for 15-20 hours under the condition of micro vacuum or normal pressure to obtain a crude product; s2, post-processing: adding a proper amount of acid into a reaction system for neutralization, vacuumizing the reactor after the neutralization is finished, heating to 80-100 ℃ for removing residual methanol and unreacted dimethyl carbonate, continuously heating to 160-180 ℃ and distilling to obtain a 3-trimethoxy silane methyl carbamate product. The reaction raw materials selected by the invention are all widely and easily available, the quality is controllable, and the raw materials are all low-toxicity chemicals, so that the use of high-toxicity, extremely-toxic, flammable and explosive chemicals is avoided.
Description
Technical Field
The invention relates to the field of organosilicon chemical intermediates, in particular to a preparation method of 3-trimethoxysilane methyl carbamate.
Background
The main purpose of the silane coupling agent is that (1) surface treatment: the adhesive property of glass fiber and resin can be improved; (2) Plastic filling: the dispersibility and the adhesive force of the filler in the resin can be improved, and the compatibility between the inorganic filler and the resin can be improved; (3) adhesion promoters for use as sealants, adhesives and coatings: can improve the bonding strength, water resistance, weather resistance and other performances.
The 3-trimethoxy silane methyl carbamate is not only a silane coupling agent, but also can be used as an intermediate for preparing isocyanate coupling agent (3-isocyanatopropyl trimethoxy silane), the latter is an important coupling agent, and is widely used for high-grade polyurethane sealant and modified polyurethane resin, and can also be used as a tackifier of room temperature vulcanized silicone rubber, a constituent component of varnish resin and the like. Therefore, 3-trimethoxysilane methyl carbamate is a special chemical and has special effect in the field of silane coupling agents.
There are few reports on the preparation method of the chemical in China at present, and the application is made based on the reports.
Disclosure of Invention
In view of the background art, the invention aims to provide a preparation method of a silane coupling agent, namely 3-trimethoxysilane methyl carbamate.
The invention aims at realizing the following technical scheme:
the preparation method of the 3-trimethoxysilane methyl carbamate comprises the following steps:
s1, sequentially adding raw materials of aminosilane, dimethyl carbonate (DMC) and a catalyst into a reactor, wherein the molar ratio of the aminosilane to the dimethyl carbonate is 2:1-4:1, introducing nitrogen into the reactor to replace and discharge air, heating a reaction system to 90-115 ℃ under the condition of stirring, preserving heat under the condition of micro vacuum or normal pressure, and reacting for 15-20 hours, wherein the reaction equation is as follows:
obtaining a crude product;
s2, adding a proper amount of acid into the reactor for neutralization, vacuumizing the reactor after the neutralization is finished, heating to 80-100 ℃ for removing residual methanol and unreacted dimethyl carbonate, continuously heating to 160-180 ℃ and distilling to obtain a 3-trimethoxy silane methyl carbamate product.
In the step S1, the reaction materials, namely the raw materials, are sensitive to water, and the reaction kettle is ensured to be clean, dried, anhydrous and filled with nitrogen for standby before feeding.
In the step S1, the chemical name of the raw material aminosilane is aminopropyl trimethoxysilane, and the chemical structural formula is as follows:
further, the catalyst in S1 is a base catalyst, such as an inorganic base: sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium phosphate, or the like; or an organic base: triethylamine, trimethylamine, triphenylphosphine, n-butyllithium, tetramethylammonium hydroxide, tetrabutylammonium hydroxide, triethanolamine or isopropanol alcohol amine.
Further, in the step S1, if inorganic base is used as a catalyst, stirring is sufficiently and uniformly performed, and the stirring speed is controlled to be 400-500 rpm/min.
Furthermore, in the reaction process in the step S1, the byproduct methanol is required to be timely discharged, a condensation reflux device is arranged at the top of the reaction kettle, and the reaction materials can be condensed and refluxed while the methanol is discharged.
Further, the acid used for neutralizing the reaction mass in S2 may be sulfuric acid, hydrochloric acid, glacial acetic acid, lactic acid, propionic acid or butyric acid.
Further, a preferable technical scheme is as follows: the molar ratio of the aminosilane to the dimethyl carbonate is more suitable for 2.1:1-2.5:1, the catalyst inorganic base is more suitable for sodium hydroxide (the addition amount is 1-1.4%), the potassium hydroxide (the addition amount is 0.7-1%), and the organic base is more suitable for triethylamine (the addition amount is 1.4-1.8%). The reaction temperature is more suitable at 90-100 ℃, the reaction time is more suitable at 15-17 h, and sulfuric acid or glacial acetic acid is more suitable for neutralization after the reaction is finished.
Compared with the prior art, the invention has the following advantages:
(1) The reaction raw materials selected by the invention are all widely and easily available, the quality is controllable, and the raw materials are all low-toxicity chemicals, so that the use of high-toxicity, extremely-toxic, flammable and explosive chemicals is avoided;
(2) The invention avoids the use of solvent, omits the steps of solvent separation and recovery, has simple required equipment, does not have complex procedures and dangerous operation;
(3) Under the preferable condition of the invention, the conversion rate of the raw material aminosilane can reach 100 percent, and the unreacted part of dimethyl carbonate can be recovered and reused. The obtained product has high yield and light color.
Detailed Description
The present invention will be described in further detail with reference to the following specific embodiments.
In the following examples and comparative examples, materials, reagents and instruments used were obtained commercially or materials, reagents therein were prepared by conventional methods unless otherwise specified.
Example 1:
providing the following raw materials: six parts of aminosilane (179 g each), six parts of dimethyl carbonate (200 g each), two parts of sodium hydroxide (3.8 g, 4.5g respectively), two parts of potassium hydroxide (2.8 g, 3.8g respectively), two parts of triethylamine (5.3 g, 6g respectively) were weighed out: two parts of sodium hydroxide, two parts of potassium hydroxide and two parts of triethylamine form six parts of catalysts together; the raw materials are divided into six groups, and each group comprises 179g of aminosilane, 200g of dimethyl carbonate and one catalyst;
providing a reaction kettle, ensuring that the reaction kettle is clean, dry and anhydrous before feeding, and filling nitrogen for later use, wherein a condensation reflux device is arranged at the top of the reaction kettle, and performing six groups of parallel experiments, wherein each group of experiments comprises the following steps:
a group of raw materials are put into a reaction kettle, specifically, raw materials of aminosilane, dimethyl carbonate and a catalyst are put into a reactor in sequence, nitrogen is introduced into the reactor to replace exhaust air, the reaction system is heated to 100 ℃ under the condition of stirring, the temperature is kept, a condensation reflux device is arranged at the top of the reaction kettle, and the reaction is carried out for 16 hours under the condition of micro vacuum or normal pressure, so that a crude product is obtained.
The reaction results of the obtained crude product were analyzed by gas chromatography as follows:
table 1 influence of different catalysts on the reaction effect.
As can be seen from Table 1, the three catalysts preferred in this example perform well in the respective preferred addition ranges, and the conversion and selectivity of the crude product obtained are within the industrially acceptable range.
Example 2:
weighing six groups of raw materials, wherein each group comprises: 179g of aminosilane, 200g of dimethyl carbonate and 2.8g of potassium hydroxide, the working principle of this example is the same as that of example 1, except that: the reaction results were examined at different reaction temperatures, and the other operating conditions were the same as in example 1, and the specific reaction results are shown in Table 2.
TABLE 2 influence of different reaction temperatures on the reaction effect
As can be seen from Table 2, the conversion rate increases with increasing reaction temperature in the selected temperature range, the selectivity peaks at 90-100℃and then the selectivity decreases continuously, since the 3-trimethoxysilane methyl carbamate product is more reactive and the increase in temperature results in the product polymerizing itself to produce dimers and polymers with a substantial increase in byproducts. Thus, it can be seen that 100 ℃ is the most preferred reaction temperature.
Example 3:
weighing six groups of raw materials, wherein each group comprises: 179g of aminosilane, 200g of dimethyl carbonate and 2.8g of potassium hydroxide, the working principle of this example is the same as that of example 1, except that: the reaction results were examined at different reaction times, and other operating conditions were the same as in example 1, and specific reaction results are shown in Table 3.
TABLE 3 influence of different reaction times on the reaction effect
As can be seen from Table 3, the esterification reaction of the present invention requires a long period of time, and the conversion and selectivity peak at about 16 hours, so 16 hours is the most preferable reaction time.
Example 4:
the reaction process is discussed with respect to examples 1-3, which focus on the post-treatment process.
895g of aminosilane, 1000g of dimethyl carbonate and 14g of potassium hydroxide are weighed, the reaction operation conditions are the same as those of the example 1, after the reaction is finished, the reaction materials are divided into five groups for standby, and are respectively neutralized by sulfuric acid, hydrochloric acid, glacial acetic acid and lactic acid, and the other group is not neutralized by acid to be used as blank comparison. After neutralization, vacuumizing and heating to 90 ℃ to remove residual methanol and unreacted dimethyl carbonate, heating to 170 ℃ and distilling to obtain a 3-trimethoxysilane methyl carbamate product, wherein the specific results are shown in table 4.
TABLE 4 influence of the amount of ammonia on the catalytic amination effect of polyetheramines
As can be seen from Table 4, the crude product before the end of the reaction was distilled and refined was subjected to acid neutralization, and the direct distillation without neutralization resulted in a significant decrease in the final yield of the product. It can be seen that sulfuric acid and glacial acetic acid in the acid are more suitable.
The foregoing is a further detailed description of the provided technical solution in connection with the preferred embodiments of the present invention, and it should not be construed that the specific implementation of the present invention is limited to the above description, but it should be understood that the simple deduction and substitution made by those skilled in the art without departing from the concept of the present invention are all to be considered as falling within the scope of the present invention.
Claims (5)
1. The preparation method of the 3-trimethoxysilane methyl carbamate is characterized by comprising the following steps of:
s1, a reaction process: the method comprises the steps of sequentially adding raw materials of 3-aminopropyl trimethoxy silane, dimethyl carbonate and a catalyst into a reactor, wherein the molar ratio of 3-aminopropyl trimethoxy silane to dimethyl carbonate is 1:2.22, introducing nitrogen into the reactor to replace exhaust air, heating the reaction system to 90-115 ℃ under the condition of stirring, and reacting for 15-20 hours under the condition of normal pressure, wherein the reaction equation is as follows:
obtaining a crude product;
s2, post-processing: adding a proper amount of acid into a reaction system for neutralization, vacuumizing the reactor after the neutralization is finished, heating to 80-100 ℃ for removing residual methanol and unreacted dimethyl carbonate, continuously heating to 160-180 ℃ and distilling to obtain a 3-trimethoxy silane methyl carbamate product;
the catalyst is inorganic base: sodium hydroxide or potassium hydroxide, or an organic base: triethylamine;
when the catalyst is sodium hydroxide, the addition amount is 1% -1.4%; when the catalyst is potassium hydroxide, the addition amount is 0.7% -1%; when triethylamine is selected as the catalyst, the addition amount is 1.4% -1.8%.
2. The method according to claim 1, wherein when the catalyst is an inorganic base, the stirring in S1 is sufficiently uniform, and the stirring speed is 400 to 500rpm/min.
3. The process according to claim 1, wherein the reaction temperature in S1 is 90 to 100 ℃ and the reaction time is 15 to 17 hours.
4. The method according to claim 1, wherein the acid in S2 is sulfuric acid, hydrochloric acid, glacial acetic acid, lactic acid, propionic acid or butyric acid.
5. The method according to any one of claims 1 to 4, wherein a condensing reflux device is disposed at the top of the reactor in S1, and is used for timely discharging byproduct methanol and condensing reflux of the reaction materials in the reactor during the reaction of S1.
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| CN110317225A (en) * | 2018-03-28 | 2019-10-11 | 赢创德固赛有限公司 | The method for being used to prepare the isocyanates containing alkoxysilane groups |
| CN110317222A (en) * | 2018-03-28 | 2019-10-11 | 赢创德固赛有限公司 | The method for being used to prepare the isocyanates containing alkoxysilane groups |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102013218972A1 (en) * | 2013-09-20 | 2015-03-26 | Wacker Chemie Ag | Process for the preparation of carbamatoorganosilanes |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6673954B1 (en) * | 2003-02-19 | 2004-01-06 | General Electric Company | Process for the preparation of N-silylorganocarbamates |
| CN106488922A (en) * | 2014-07-14 | 2017-03-08 | 莫门蒂夫性能材料股份有限公司 | The manufacture method of the isocyanatoorganosilanes of low colourity and colour stable and derived from it product |
| CN110317225A (en) * | 2018-03-28 | 2019-10-11 | 赢创德固赛有限公司 | The method for being used to prepare the isocyanates containing alkoxysilane groups |
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