KR100535441B1 - The method of preparation of Isobutyltrialkoxysilane - Google Patents
The method of preparation of Isobutyltrialkoxysilane Download PDFInfo
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Abstract
본 발명은 이소부틸트리알콕시실란의 제조방법에 관한 것으로서, 더욱 상세하게는 조촉매를 고압 반응기에 투입하고 실란에 백금 촉매를 녹여서 반응기에 투입한 다음, 저온에서 메틸알켄을 상기 반응기에 투입하고, 반응기 온도를 올려 반응을 진행시킨 뒤 종료하여 반응기의 온도를 낮추고 메틸알켄을 회수한 다음 감압 증류를 이용하여 부반응물을 제거하고 이소부틸트리알콕시실란을 수득함으로써 부반응을 줄이고 중화 공정을 필요로 하지 않으면서 이소부틸트리알콕시실란을 다량 얻을 수 있는 이소부틸트리알콕시실란의 제조방법에 관한 것이다. The present invention relates to a method for producing isobutyltrialkoxysilane, and more particularly, a cocatalyst is added to a high pressure reactor, a platinum catalyst is dissolved in silane, and then charged into the reactor, and methylalkene is introduced into the reactor at a low temperature. After raising the reactor temperature to proceed with the reaction, the reaction is completed to lower the temperature of the reactor, and to recover methylalkene, and then to remove the side reactions by distillation under reduced pressure and to obtain isobutyltrialkoxysilane to reduce side reactions and to avoid the need for neutralization process The present invention relates to a method for producing isobutyltrialkoxysilane in which a large amount of isobutyltrialkoxysilane can be obtained.
Description
본 발명은 이소부틸트리알콕시실란의 제조방법에 관한 것으로서, 더욱 상세하게는 조촉매를 고압 반응기에 투입하고 실란에 백금 촉매를 녹여서 반응기에 투입한 다음, 저온에서 메틸알켄을 상기 반응기에 투입하고, 반응기 온도를 올려 반응을 진행시킨 뒤 종료하여 반응기의 온도를 낮추고 메틸알켄을 회수한 다음 감압 증류를 이용하여 부반응물을 제거하고 이소부틸트리알콕시실란을 수득함으로써 부반응을 줄이고 중화 공정을 필요로 하지 않으면서 이소부틸트리알콕시실란을 다량 얻을 수 있는 이소부틸트리알콕시실란의 제조방법에 관한 것이다. The present invention relates to a method for producing isobutyltrialkoxysilane, and more particularly, a cocatalyst is added to a high pressure reactor, a platinum catalyst is dissolved in silane, and then charged into the reactor, and methylalkene is introduced into the reactor at a low temperature. After raising the reactor temperature to proceed with the reaction, the reaction is completed to lower the temperature of the reactor, and to recover methylalkene, and then to remove the side reactions by distillation under reduced pressure and to obtain isobutyltrialkoxysilane to reduce side reactions and to avoid the need for neutralization process The present invention relates to a method for producing isobutyltrialkoxysilane in which a large amount of isobutyltrialkoxysilane can be obtained.
기존의 이소부틸트리에톡시실란의 제조방법으로는 반응성 실란을 n당량의 에틸 알코올과 반응시키는 것으로 이 방법에서는 반응 완결을 위해서 발생한 염화수소를 감압하에서 에틸 알코올과 함께 제거하고 남은 염화수소는 소량의 소듐 에톡사이드 또는 마그네슘 에톡사이드를 투입해 제거하는 방법으로 중화시 생성되는 염의 양이 적고 용제를 사용하지 않아도 되는 반면, 염화수소를 제거해주어야 하며 필터를 해야하고, 염화수소의 부식성으로 인해 고가의 감압 펌프 또는 염화수소 스크러빙 장치가 필요하며, 반응 원료인 이소부틸트리클로로실란을 합성하기가 어려운 단점을 갖고 있다[미국 특허 제 6,242,628호].Conventional method for preparing isobutyltriethoxysilane is to react a reactive silane with n equivalents of ethyl alcohol. In this method, hydrogen chloride generated to complete the reaction is removed together with ethyl alcohol under reduced pressure, and the remaining hydrogen chloride is a small amount of sodium ethoxide. Alternatively, by removing magnesium ethoxide, the amount of salt produced during neutralization is small and no solvent is used, while hydrogen chloride must be removed and filtered. Expensive decompression pump or hydrogen chloride scrubbing device is required due to the corrosion of hydrogen chloride. Is required, and it is difficult to synthesize isobutyltrichlorosilane, which is a reaction raw material (US Pat. No. 6,242,628).
이에, 본 발명자들은 상기의 문제점을 해결하기 위하여 연구한 결과, 촉매와 조촉매의 사용으로 부반응물의 생성을 낮추어 반응 수율을 높이고 중화공정을 필요로 하지 않는 이소부틸트리알콕시실란의 제조방법을 개발함으로써 본 발명을 완성하게 되었다.Accordingly, the present inventors have studied to solve the above problems, and as a result, the production of isobutyltrialkoxysilane that reduces the production of side reactions by using a catalyst and a promoter to increase the reaction yield and does not require a neutralization process Thus, the present invention has been completed.
따라서, 본 발명은 수율이 향상된 이소부틸트리알콕시실란의 제조방법을 제공하는데 그 목적이 있다. Accordingly, an object of the present invention is to provide a method for producing isobutyltrialkoxysilane with improved yield.
본 발명은The present invention
1) 다음 화학식 4로 표시되는 조촉매를 질소 기류 하에서 60 ∼ 120 분동안 건조시킨 후, 다음 화학식 1로 표시되는 실란과 다음 화학식 3으로 표시되는 촉매를 혼합하는 단계;1) drying the promoter represented by the following formula (4) for 60 to 120 minutes under a stream of nitrogen, and then mixing the silane represented by the following formula (1) and the catalyst represented by the following formula (3);
2) 반응기 온도를 0 ∼ 10 ℃로 낮추어 다음 화학식 2로 표시되는 메틸알켄을 반응기에 투입하는 단계;2) lowering the reactor temperature to 0 to 10 ° C. and then introducing methylalkene represented by Formula 2 into the reactor;
3) 반응기 온도를 50 ∼ 150 ℃까지 높이고 12 ∼ 24시간동안 반응기를 교반시하는 단계;3) raising the reactor temperature to 50-150 ° C. and stirring the reactor for 12-24 hours;
4) 반응기 온도를 10 ∼ 25 ℃로 낮추어 미반응물인 과량의 메틸알켄을 회수하고 감압증류하여 이소부틸트리알콕시실란을 수득하는 단계로 이루어진 이소부틸트리알콕시실란의 제조방법을 그 특징으로 한다.4) A method for producing isobutyltrialkoxysilane consisting of recovering excess methylalkene as an unreacted product by distilling under reduced pressure to obtain isobutyltrialkoxysilane by reducing the reactor temperature to 10 to 25 ° C.
상기 화학식 1에서 R1은 탄소수 1 이상의 알킬기이며, 바람직한 상기 화학식 1로 표시되는 화합물로는 트리메톡시실란, 트리에톡시실란, 트리프로톡시실란, 트리부톡시실란 등이 있다.In Formula 1, R 1 is an alkyl group having 1 or more carbon atoms, and preferred compounds represented by Formula 1 include trimethoxysilane, triethoxysilane, triprooxysilane, and tributoxysilane.
상기 화학식 2에서; R2은 탄소수 1 ∼ 4개의 알킬기를 나타낸다. 바람직하기로는 2-메틸프로펜, 2-메틸부텐, 2-메틸펜텐 등이 있다.In Chemical Formula 2; R <2> represents a C1-C4 alkyl group. Preferred are 2-methylpropene, 2-methylbutene, 2-methylpentene and the like.
상기 화학식 3에서; R3은 비닐기, R4는 메틸기 또는 에틸기를 나타낸다. 바람직하기로는 플라티눔(0)-1,3-디비닐-1,1,3,3,테트라메틸디실록산 복합체, 플라티눔(0)-1,3-디비닐-1,1,3,3,테트라에틸디실록산 복합체 등이 있다In Chemical Formula 3; R <3> represents a vinyl group and R <4> represents a methyl group or an ethyl group. Preferably platinum (0) -1,3-divinyl-1,1,3,3, tetramethyldisiloxane complex, platinum (0) -1,3-divinyl-1,1,3,3 And tetraethyldisiloxane complexes.
상기 화학식 4에서; M은 K 또는 Na이다.In Chemical Formula 4; M is K or Na.
이와 같은 본 발명을 더욱 상세하게 설명하면 다음과 같다. The present invention will be described in more detail as follows.
1) 단계에서는 조촉매로 상기 화학식 4로 표시되는 화합물을 사용하여 건조된 반응기에 투입하고 반응기를 질소로 60 ∼ 120분, 바람직하게는 80 ∼ 100분에 걸쳐 건조시키고, 상기 화학식 1로 표시되는 실란과, 상기 화학식 3으로 표시되는 촉매를 혼합하여 투입한다. 상기 조촉매는 실란 100 중량부에 대하여 1 ∼ 3 중량부, 바람직하게는 1.2 ∼ 1.6 중량부를 사용하며, 상기 촉매는 실란 100 중량부에 대하여 3 ∼ 5 중량부, 바람직하게는 3.5 ∼ 4.5 중량부를 사용한다. 이때 조촉매를 1 중량부 미만으로 사용하면 반응수율이 감소하는 문제점이 있고, 3 중량부 초과하여 사용하면 반응후 제거해야 할 조촉매가 많아지는 문제가 있다. 또한, 촉매 3 중량부 미만 사용할 경우에는 반응속도가 느려지는 문제점이 있고, 5 중량부를 초과하면 원가가 상승하는 문제가 있다. 한편, 상기 건조시간이 60분 미만일 경우에는 부반응이 진행되는 문제가 있으며, 120분을 초과할 경우에는 생산성이 저하되는 문제점이 있다.In step 1), a promoter is added to a dried reactor using a compound represented by Chemical Formula 4, and the reactor is dried with nitrogen for 60 to 120 minutes, preferably 80 to 100 minutes, and is represented by Chemical Formula 1 The silane and the catalyst represented by the formula (3) are mixed and added. The promoter is used in an amount of 1 to 3 parts by weight, preferably 1.2 to 1.6 parts by weight, based on 100 parts by weight of silane, and the catalyst is 3 to 5 parts by weight, preferably 3.5 to 4.5 parts by weight, based on 100 parts by weight of silane. use. In this case, if the amount of the promoter is less than 1 part by weight, the reaction yield is reduced. If the amount is more than 3 parts by weight, the amount of promoter to be removed after the reaction is increased. In addition, when using less than 3 parts by weight of the catalyst there is a problem that the reaction rate is slow, and if more than 5 parts by weight there is a problem that the cost rises. On the other hand, if the drying time is less than 60 minutes, there is a problem that the side reaction proceeds, if it exceeds 120 minutes there is a problem that the productivity is lowered.
2) 단계에서는 반응기의 온도를 0 ∼ 10 ℃, 바람직하게는 0 ∼ 5 ℃로 낮추어 상기 화학식 2로 표시되는 메틸알켄을 투입한다. 이때, 상기 메틸알켄의 함유량은 상기 실란 100 중량부에 대하여 70 ∼ 300 중량부가 바람직하며, 110 ∼ 180 중량부가 더욱 바람직하다. 만일 상기 메틸알켄이 70 중량부 미만이면 반응속도가 느려지는 문제점이 있고, 300 중량부 초과하면 회수해야할 메틸알켄이 많아지는 문제점이 있다. 또한, 저온으로 반응기 온도를 낮출 때 0 ℃ 미만으로 낮추면 메틸알켄이 액화되어 투입이 느려지는 문제점이 있고, 10 ℃를 초과하면 기체인 메틸알켄의 투입이 어려운 문제점이 있다.In step 2), the temperature of the reactor is reduced to 0 to 10 ° C., preferably 0 to 5 ° C., to add methylalkene represented by Chemical Formula 2. At this time, 70-300 weight part is preferable with respect to 100 weight part of said silane, and, as for content of the said methyl alkene, 110-180 weight part is more preferable. If the methyl alken is less than 70 parts by weight, there is a problem that the reaction rate is slow, and if it exceeds 300 parts by weight, there is a problem that the methyl alken to be recovered increases. In addition, when lowering the reactor temperature at a low temperature to lower than 0 ℃ methyl alkene is liquefied and there is a problem that the input is slow, if it exceeds 10 ℃ there is a problem that the addition of methyl alkene gas is difficult.
3) 단계에서는 반응기의 온도를 50 ∼ 150 ℃, 바람직하게는 110 ∼ 130 ℃ 까지 높이고 반응기를 교반시켜 준다. 반응시간으로는 12 ∼ 24시간, 바람직하게는 14 ∼ 18시간이 적당하다. 이때 반응 온도를 50 ℃ 미만일 경우에는 반응속도가 느려지는 문제점이 있고, 150 ℃ 초과하면 과다한 가열로 인한 열손실이 발생하는 문제점이 있다. 또한, 반응시간이 12 시간 미만일 경우에는 반응수율이 저하되는 문제점 있고, 24시간 초과할 경우에는 부반응이 진행되는 문제점이 있다.In step 3), the temperature of the reactor is increased to 50 to 150 ° C, preferably 110 to 130 ° C, and the reactor is stirred. As reaction time, 12 to 24 hours, Preferably 14 to 18 hours are suitable. At this time, when the reaction temperature is less than 50 ℃ there is a problem that the reaction rate is slow, if it exceeds 150 ℃ there is a problem that heat loss due to excessive heating occurs. In addition, if the reaction time is less than 12 hours, there is a problem that the reaction yield is lowered, if more than 24 hours there is a problem that the side reaction proceeds.
4) 단계에서는 10 ∼ 25 ℃로 온도를 낮추어 미반응물인 과량의 메틸알켄을 반응기로부터 회수하고 감압 증류를 통해 이소부틸트리알콕시실란을 분리하는 단계이다. 이때 온도를 10 ℃ 미만으로 낮추면 메틸알켄의 회수가 어려우며, 생산성 저하의 문제점이 있고, 25 ℃ 초과하면 메틸알켄으로 인하여 반응기 내의 압력이 증가하는 문제점이 있다. 또한, 회수되는 메틸알켄은 다시 이소부틸트리알콕시실란 제조에 재사용할 수 있다.In step 4), the temperature is lowered to 10 to 25 ° C. to recover excess methylalkene, an unreacted substance, from the reactor, and isobutyltrialkoxysilane is separated by distillation under reduced pressure. At this time, if the temperature is lowered below 10 ℃, it is difficult to recover the methyl alkenes, there is a problem of lowering the productivity, if the temperature exceeds 25 ℃ there is a problem that the pressure in the reactor increases due to the methyl alkenes. In addition, the methylalkene recovered can be reused for the production of isobutyltrialkoxysilane.
본 발명에 있어서 반응의 합성 여부는 통상적 방법, 즉 가스크로마토그래피, 질량 분석기, 적외선 분광기 및 핵자기 공명 분석기 등을 사용하여 확인한다. 합성의 정도는 반응기에 장착된 압력계의 변화를 통해 알 수 있었다.In the present invention, the synthesis of the reaction is confirmed using conventional methods, ie, gas chromatography, mass spectrometry, infrared spectroscopy, and nuclear magnetic resonance analyzer. The degree of synthesis was determined by changes in the pressure gauge mounted on the reactor.
이와 같은 이소부틸트리알콕시실란의 제조방법은 중화 및 필터 공정을 필요로 하지 않는 촉매반응을 진행시키는 한편, 촉매와 조촉매를 사용함으로써 부반응물의 생성을 줄이고 이소부틸트리알콕시실란을 다량 얻을 수 있다. Such a method for producing isobutyltrialkoxysilane proceeds with a catalytic reaction that does not require a neutralization and filter process, while reducing the formation of side reactions and obtaining a large amount of isobutyltrialkoxysilane by using a catalyst and a promoter. .
이하, 본 발명은 다음 실시예에 의거하여 더욱 상세히 설명하겠는바, 본 발명이 이에 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail based on the following examples, but the present invention is not limited thereto.
실시예 1Example 1
온도계, 압력계, 노즐, 교반 장치가 설치되어 있고, 멘틀이 연결되어 있는 500 ㎖ 고압 반응기에 조촉매인 소듐 카보네이트(Na2CO3) 0,56 g을 투입한 후, 질소를 불어주면서 반응기에 수분과 산소를 제거하였다. 1시간 동안 질소를 불어준 다음 반응성 실란인 트리에톡시실란 40 g과 촉매인 플래티늄(0)-1,3-디비닐-1,1,3,3,-테트라메틸디실록산 착물 1.57 g을 섞어 투입하였다. 반응기의 온도를 0 ℃까지 낮춘 뒤 2-메틸프로핀 41 g을 투입한 다음 온도를 130 ℃까지 올렸다. 반응 시간 12시간 뒤 압력이 떨어졌고, 온도를 20 ℃로 낮춘 뒤 미반응물 2-메틸프로핀을 회수한 다음 생성물을 감압 증류하였다. 이소부틸트리에톡시실란 42.9 g을 얻었고 수율은 80%였다. 부반응물인 테트라에톡시실란은 5.6 g(11%)을 얻었다.0,56 g of sodium carbonate (Na 2 CO 3 ), a cocatalyst, was added to a 500 ml high-pressure reactor equipped with a thermometer, pressure gauge, nozzle, and stirring device, and then water was added to the reactor while blowing nitrogen. And oxygen were removed. After nitrogen blowing for 1 hour, 40 g of triethoxysilane, a reactive silane, and 1.57 g of platinum (0) -1,3-divinyl-1,1,3,3, -tetramethyldisiloxane complex were mixed. Input. After the temperature of the reactor was lowered to 0 ° C., 41 g of 2-methylpropene was added thereto, and the temperature was raised to 130 ° C. After 12 hours of reaction time, the pressure dropped, and after the temperature was lowered to 20 ° C., unreacted 2-methylpropine was recovered, and the product was distilled under reduced pressure. 42.9 g of isobutyltriethoxysilane were obtained and the yield was 80%. As a side reaction, tetraethoxysilane obtained 5.6 g (11%).
실시예 2Example 2
트리메톡시실란 30 g을 사용한 것 이외에는 상기 실시예 1과 동일한 방법으로 13시간 130 ℃에서 반응시켜 이소부틸트리메톡시실란을 제조하였다. 수율은 81%로 35.4 g을 얻었고 부반응물 테트라메톡시실란 3.7 g(10%)을 얻었다. Except that 30 g of trimethoxysilane was used, the reaction was carried out at 130 ° C. for 13 hours in the same manner as in Example 1 to prepare isobutyltrimethoxysilane. Yield was 35.4 g at 81% and 3.7 g (10%) of the side reaction tetramethoxysilane.
비교예 1Comparative Example 1
온도계, 적가장치, 콘덴서, 스크러버가 설치된 500 ㎖ 3구 라운드 플라스크에 이소부틸트리클로로실란 100 g을 투입한 후 마그네틱 스터러로 천천히 교반함과 동시에 얼음 중탕을 사용하여 3 ℃로 유지하면서 에탄올 80 g을 적가 장치를 통해 천천히 2시간 동안 적가하였다. 적가도중 생성된 염화수소는 기체유도관을 통해 스크러버로 이동하였다. 적가가 끝난 다음 반응 혼합물을 5 ℃에서 1시간 반응시켰다. 이때 150 torr로 감압하여 기체 염화수소를 스크러빙 장치로 유도, 제거하였다. 생성물에 소듐 에톡사이드(30% 에탄올 용액) 28.2 g을 적가시켜 중화시킨 다음 침전된 소듐 클로라이드를 여과시켰다. 증류하여 에탄올을 제거한 뒤 승온 감압 증류하여 이소부틸트리에톡시실란 97.8 g을 얻었다. 생성된 염인 소듐 클로라이드는 9.2 g이었고 수율은 82%이었다.100 g of isobutyltrichlorosilane was added to a 500 ml three-necked round flask equipped with a thermometer, a dropping device, a condenser, and a scrubber. The mixture was stirred slowly with a magnetic stirrer and kept at 3 ° C using an ice bath. Was added slowly through the dropping device for 2 hours. Hydrogen chloride produced during the dropping was transferred to the scrubber through a gas induction pipe. After completion of the dropwise addition, the reaction mixture was reacted at 5 ° C for 1 hour. At this time, the pressure was reduced to 150 torr to guide and remove the gaseous hydrogen chloride with a scrubbing device. The product was neutralized by dropwise addition of 28.2 g of sodium ethoxide (30% ethanol solution) and the precipitated sodium chloride was filtered off. Distillation removed ethanol, and distillation under reduced pressure was carried out to obtain 97.8 g of isobutyltriethoxysilane. The resulting salt, sodium chloride, was 9.2 g and yield was 82%.
비교예 2Comparative Example 2
소듐 카보네이트를 사용하지 않은 것 이외에는 상기 실시예 1과 동일한 방법으로 반응시켜 이소부틸트리메톡시실란을 제조하였다. 수율은 60%로 32.2 g을 얻었고 부반응물 테트라메톡시실란 11.1 g(30%)을 얻었다.Except not using sodium carbonate, the reaction was carried out in the same manner as in Example 1 to prepare isobutyltrimethoxysilane. The yield was 32.2 g at 60% and 11.1 g (30%) of the side reaction tetramethoxysilane.
상기의 본 발명에 따른 실시예와 종래 비교예에 의한 실란의 제조방법을 비교해 보면 비교예 1의 경우 중화공정이 필요하고, 과량의 에탄올을 증류해야 하는 단점이 있으며, 중화제로 들어가는 소듐 에톡사이드는 당량 이상이 들어가야 완벽히 염화수소를 제거할 수 있으므로 중화 후 잔존하는 소듐 에톡사이드가 증류 시 수분에 의해 강염기가 되어 트리메톡시실란이 가수분해가 될 수 있는 단점이 있다. 또한, 비교예 2의 경우 조촉매(소듐 카보네이트)를 첨가하지 않아서, 수율이 크게 적어 졌다.Comparing the production method of the silane according to the embodiment according to the present invention and the conventional comparative example in the case of Comparative Example 1, the neutralization step is required, there is a disadvantage that distillation of excess ethanol, sodium ethoxide to enter the neutralizing agent Hydrogen chloride can be completely removed only when the equivalent is present, so that sodium ethoxide remaining after neutralization becomes a strong base by water during distillation, and trimethoxysilane can be hydrolyzed. In addition, in the case of the comparative example 2, the cocatalyst (sodium carbonate) was not added and the yield fell large.
반면, 실시예 1 ∼ 2의 경우에는 조촉매 사용으로 부반응물의 발생을 줄여서 수율을 크게 향상시킬 수 있었다. On the other hand, in the case of Examples 1 to 2 it was possible to greatly improve the yield by reducing the occurrence of side reactions by using a promoter.
이상에서 상세히 설명하였듯이, 본 발명에 따른 이소부틸트리알콕시실란의 제조방법은 중화 공정이 필요없는 촉매반응을 진행시키는 한편, 촉매와 조촉매를 사용함으로써 부반응물의 생성을 줄이고 이소부틸트리알콕시실란을 다량 얻을 수 있는 장점이 있다. 이렇게 얻어진 이소부틸트리알콕시실란은 콘크리트용 발수제 등으로 유용하다.As described in detail above, the method for preparing isobutyltrialkoxysilane according to the present invention proceeds with a catalytic reaction that does not require a neutralization step, while reducing the formation of side reactions by using a catalyst and a promoter and reducing isobutyltrialkoxysilane. There is an advantage that can be obtained in large quantities. The isobutyltrialkoxysilane thus obtained is useful as a water repellent for concrete and the like.
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