A method for extracting methyl tributylidene oxime silane

Abstract

The present invention provides a method for extracting methyl tributylacetoximate silane, belonging to the technical field of oxime silane extraction. Specifically, a mixture of methyl tributylacetoximate silane and a solvent is prepared from methyl trichlorosilane, butanone oxime and 120# solvent gasoline raw materials, and the solvent and unreacted butanone oxime are evaporated by a thin film evaporator to obtain a methyl tributylacetoximate silane finished product; in addition, the present invention provides an extraction synergist, which effectively improves the extraction efficiency of a turbo extraction tower, further improves the raw material utilization rate, and reduces production losses.

Description

Technical Field

[0001] The invention relates to the technical field of oxime silane extraction, in particular to a method for extracting methyl tributylacetoxiime silane. Background Art

[0002] Methyl tributyl ketoxime silane is a common organosilicon crosslinking agent. Its main body is a colorless or light yellow transparent liquid. It is mainly used in the production of room temperature vulcanized silicone rubber and neutral silicone glass glue. Methyl tributyl ketoxime silane is generally produced by the reaction of methyl trichlorosilane and butanone oxime in 120# solvent oil. When methyl trichlorosilane and butanone oxime react to produce methyl tributyl ketoxime silane, butanone oxime hydrochloride will also be produced as a by-product. Since butanone oxime hydrochloride has the physical property of high viscosity, the generated butanone oxime hydrochloride will contain some (2% to 5%) methyl tributyl ketoxime silane.

[0003] CN201811502081.X relates to a method for preparing a silane crosslinking agent, and in particular to a method for preparing methyl tributylanoxime silane. The method for preparing methyl tributylanoxime silane of the present invention comprises the following steps: butanone oxime and methyl trichlorosilane are passed into a reactor, reacted at 55-65°C under normal pressure for 1-2 hours, and the reacted material is passed into a separation section for separation; the molar ratio of butanone oxime to methyl trichlorosilane is 6:1; the upper material after separation enters a neutralizer, and butanone oxime hydrochloride in the upper material is neutralized with ammonia, and the neutralized material is subjected to liquid-solid separation, the solid is dried to obtain ammonium chloride, and the liquid enters an evaporator for two distillations to obtain methyl tributylanoxime silane.

[0004] CN202446857U An extraction tower for butanone oxime hydrochloride relates to the field of chemical extraction and separation. It includes an extraction tower body with a stirring device inside, a solvent discharge port at the top of the extraction tower body, a material discharge port at the bottom, a material feed port and a solvent feed port at the side of the extraction tower body, the stirring device is a turbine mixer, and a plurality of annular fixed orifice plates are vertically arranged on the inner wall of the extraction tower body.

[0005] However, in the existing public technology, in order to maximize energy utilization, butanone oxime hydrochloride and 120# solvent oil are generally mixed and stirred to extract methyltributylacetonato silane contained in butanone oxime hydrochloride. The traditional extraction device may have uneven dispersion and incomplete extraction due to the high viscosity of butanone oxime hydrochloride. Summary of the invention

[0006] 1. Technical issues to be resolved

[0007] In view of the deficiencies in the prior art, the present invention provides a method for extracting methyl tributylacetoximate silane, which achieves sufficient stirring of the liquid-liquid mixture in an extraction tower so that the methyl tributylacetoximate silane in butanone oxime hydrochloride can be fully extracted, the materials can be fully recycled, the utilization rate of the raw materials is greatly improved, and the problems in the background technology can be effectively solved.

[0008] (II) Technical solution

[0009] To achieve the above object, the technical solution adopted by the present invention is:

[0010] A method for extracting methyl tributylidene oxime silane comprises the following steps:

[0011] S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is the butanone oxime hydrochloride precipitate;

[0012] S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower;

[0013] S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling;

[0014] S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters the neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained.

[0015] Preferably, the feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.48-3.65:1.

[0016] Preferably, the temperature in S1 is 35-45°C.

[0017] Preferably, part of the material after the reaction in S1 is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

[0018] Preferably, the solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

[0019] Preferably, the feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:2-3.

[0020] Preferably, a plurality of turbines are arranged in the extraction tower in S2, and the turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

[0021] Furthermore, in order to accelerate the formation and transmission rate of butanone oxime hydrochloride precipitate, the present invention provides an extraction enhancer, the addition amount of which is 0.1-1% of 120# solvent gasoline.

[0022] Furthermore, the extraction enhancer preparation method is:

[0023] According to the mass proportions, 30-50 parts of 1-aminopropyl-3-methylimidazole nitrate and 0.001-0.1 parts of ferric acrylate are added to 300-400 parts of DMF, and after being stirred and mixed evenly, 2-5 parts of triethylamine are added, and then the mixture is stirred and reacted at room temperature for 20-40 minutes, and then 0.01-0.3 parts of acryloxysilane are added, the temperature is controlled at 50-70°C, the mixture is stirred and reacted for 10-20 minutes, and then 12-22 parts of ethylene glycol acrylate are added, the temperature is controlled at 50-70°C, the mixture is stirred and reacted for 100-120 minutes, and DMF is removed by distillation under reduced pressure to obtain an extraction enhancer.

[0024] Preferably, the acryloxysilane is selected from at least one of 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0) and 2-acrylate 3-(diethoxymethylsilyl)propyl ester (CAS No.: 13732-00-8).

[0025] Preferably, the ethylene glycol acrylate is at least one selected from ethylene glycol dimethacrylate, tetraethylene glycol dimethacrylate, and triethylene glycol dimethacrylate.

[0026] In the present invention, 1-aminopropyl-3-methylimidazole nitrate, ferric acrylate and acryloxysilane are subjected to addition reaction, and then subjected to addition reaction with ethylene glycol acrylate, and the obtained extraction enhancer can be used as a mass transfer medium to form an extractant liquid film under high-speed stirring; and is combined with a 120# solvent gasoline extractant to accelerate the formation of butanone oxime hydrochloride precipitate and the transmission rate.

[0027] (III) Beneficial effects

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] (1) The methyl tributylidene oxime silane prepared in the embodiment of the present invention has high content, high purity and high product yield;

[0030] (2) In the embodiments of the present invention, the conversion rate of the reaction raw materials is high, which makes full use of the raw materials and reduces the consumption and waste of raw materials;

[0031] (3) The extraction enhancer prepared by the addition reaction of 1-aminopropyl-3-methylimidazole nitrate, ferric acrylate and acryloxysilane in the embodiment of the present invention greatly improves the extraction rate, thereby effectively improving the product utilization rate and reducing product loss. BRIEF DESCRIPTION OF THE DRAWINGS

[0032] Figure 1 This is the chromatogram of methyl tributylacetonate oxime silane in Example 3. DETAILED DESCRIPTION

[0033] The technical scheme of the present invention is further described below by specific embodiments. Those skilled in the art should understand that the specific embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention. Unless otherwise specified, the technical means used in the following examples are conventional means well known to those skilled in the art, and the raw materials used are all commercially available conventional commodities.

[0034] <Example 1>

[0035] A method for extracting methyl tributylidene oxime silane comprises the following steps:

[0036] S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is the butanone oxime hydrochloride precipitate;

[0037] S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower;

[0038] S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling;

[0039] S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters the neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained.

[0040] The feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.48:1.

[0041] The temperature in S1 is 35°C.

[0042] After the reaction in S1, part of the material is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

[0043] The solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

[0044] The feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:2.

[0045] In the extraction tower of S2, multiple turbines are arranged. The turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

[0046] The amount of extraction enhancer added is 0.1% of 120# solvent gasoline.

[0047] The preparation method of the extraction enhancer is:

[0048] 30 kg of 1-aminopropyl-3-methylimidazole nitrate and 0.001 kg of ferric acrylate are added to 300 kg of DMF, and after stirring and mixing evenly, 2 kg of triethylamine is added, and then the mixture is stirred and reacted at room temperature for 20 minutes, and then 0.01 kg of acryloxysilane is added, the temperature is controlled at 50°C, and the mixture is stirred and reacted for 20 minutes, and then 12 kg of ethylene glycol acrylate is added, the temperature is controlled at 50°C, and the mixture is stirred and reacted for 120 minutes, and DMF is removed by distillation under reduced pressure to obtain an extraction enhancer.

[0049] The acryloxysilane is selected from 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0050] The ethylene glycol acrylate is selected from ethylene glycol dimethacrylate.

[0051] After analysis and balance: the average conversion rate of the reaction raw materials is 97.4%, the content of methyl tributylacetonate oxime silane in the product is 97.88%, the extraction rate of the turbo extraction tower product is 92.7%, the yield of methyl tributylacetonate oxime silane in the reaction process is 95.5%, and the purity of the value-added product ammonium chloride is 95.8%.

[0052] <Example 2>

[0053] A method for extracting methyl tributylidene oxime silane comprises the following steps:

[0054] S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is the butanone oxime hydrochloride precipitate;

[0055] S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower;

[0056] S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling;

[0057] S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters the neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained.

[0058] The feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.55:1.

[0059] The temperature in S1 is 40°C.

[0060] After the reaction in S1, part of the material is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

[0061] The solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

[0062] The feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:2.5.

[0063] In the extraction tower of S2, multiple turbines are arranged. The turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

[0064] The amount of extraction enhancer added is 0.55% of 120# solvent gasoline.

[0065] The preparation method of the extraction enhancer is:

[0066] 40 kg of 1-aminopropyl-3-methylimidazole nitrate and 0.05 kg of ferric acrylate are added to 350 kg of DMF, and after stirring and mixing evenly, 3.5 kg of triethylamine is added, and then the mixture is stirred and reacted at room temperature for 30 minutes, and then 0.12 kg of acryloxysilane is added, the temperature is controlled at 60°C, and the mixture is stirred and reacted for 15 minutes, and then 17 kg of ethylene glycol acrylate is added, the temperature is controlled at 60°C, and the mixture is stirred and reacted for 110 minutes, and DMF is removed by distillation under reduced pressure to obtain an extraction enhancer.

[0067] The acryloxysilane is selected from 3-(diethoxymethylsilyl)propyl 2-acrylate (CAS No.: 13732-00-8).

[0068] The ethylene glycol acrylate is selected from tetraethylene glycol dimethacrylate.

[0069] After analysis and balance: the average conversion rate of the reaction raw materials is 98.3%, the content of methyl tributylacetonate oxime silane in the product is 98.21%, the extraction rate of the turbo extraction tower product is 93.6%, the yield of methyl tributylacetonate oxime silane in the reaction process is 96.1%, and the purity of the value-added product ammonium chloride is 96.2%.

[0070] <Example 3>

[0071] A method for extracting methyl tributylidene oxime silane comprises the following steps:

[0072] S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is the butanone oxime hydrochloride precipitate;

[0073] S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower;

[0074] S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling;

[0075] S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters the neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained.

[0076] The feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.65:1.

[0077] The temperature in S1 is 45°C.

[0078] After the reaction in S1, part of the material is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

[0079] The solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

[0080] The feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:3.

[0081] In the extraction tower of S2, multiple turbines are arranged. The turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

[0082] The amount of extraction enhancer added is 1% of 120# solvent gasoline.

[0083] The preparation method of the extraction enhancer is:

[0084] 50 kg of 1-aminopropyl-3-methylimidazole nitrate and 0.1 kg of ferric acrylate are added to 400 kg of DMF, and after stirring and mixing evenly, 5 kg of triethylamine is added, and then the mixture is stirred and reacted at room temperature for 40 minutes, and then 0.3 kg of acryloxysilane is added, the temperature is controlled at 70°C, and the mixture is stirred and reacted for 10 minutes, and then 22 kg of ethylene glycol acrylate is added, the temperature is controlled at 70°C, and the mixture is stirred and reacted for 100 minutes, and DMF is removed by distillation under reduced pressure to obtain an extraction enhancer.

[0085] The acryloxysilane is selected from 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0086] The ethylene glycol acrylate is selected from triethylene glycol dimethacrylate.

[0087] After analysis and balance: the average conversion rate of the reaction raw materials is 98.5%, the content of methyl tributylacetonate oxime silane in the product is 98.35%, the extraction rate of the turbo extraction tower product is 94.1%, the yield of methyl tributylacetonate oxime silane in the reaction process is 96.0%, and the purity of the value-added product ammonium chloride is 95.9%.

[0088] <Comparative Example 1>

[0089] A method for extracting methyl tributylidene oxime silane comprises the following steps:

[0090] S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is the butanone oxime hydrochloride precipitate;

[0091] S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower;

[0092] S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling;

[0093] S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters the neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained.

[0094] The feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.48:1.

[0095] The temperature in S1 is 35°C.

[0096] After the reaction in S1, part of the material is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

[0097] The solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

[0098] The feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:2.

[0099] In the extraction tower of S2, multiple turbines are arranged. The turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

[0100] After analysis and balance: the average conversion rate of the reaction raw materials is 94.4%, the content of methyl tributylacetonate oxime silane in the product is 95.85%, the extraction rate of the turbo extraction tower product is 80.2%, the yield of methyl tributylacetonate oxime silane in the reaction process is 91.1%, and the purity of the value-added product ammonium chloride is 92.5%.

[0101] <Comparative Example 2>

[0102] A method for extracting methyl tributylidene oxime silane comprises the following steps:

[0103] S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is the butanone oxime hydrochloride precipitate;

[0104] S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower;

[0105] S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling;

[0106] S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters the neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained.

[0107] The feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.48:1.

[0108] The temperature in S1 is 35°C.

[0109] After the reaction in S1, part of the material is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

[0110] The solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

[0111] The feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:2.

[0112] In the extraction tower of S2, multiple turbines are arranged. The turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

[0113] The amount of extraction enhancer added is 0.1% of 120# solvent gasoline.

[0114] The preparation method of the extraction enhancer is:

[0115] 0.001 kg of ferric acrylate is added to 300 kg of DMF, and after stirring and mixing evenly, 2 kg of triethylamine is added, and then the mixture is stirred and reacted at room temperature for 20 minutes. Then, 0.01 kg of acryloxysilane is added, the temperature is controlled at 50°C, and the mixture is stirred and reacted for 20 minutes. Then, 12 kg of ethylene glycol acrylate is added, the temperature is controlled at 50°C, and the mixture is stirred and reacted for 120 minutes. DMF is removed by vacuum distillation to obtain an extraction enhancer.

[0116] The acryloxysilane is selected from 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0117] The ethylene glycol acrylate is selected from ethylene glycol dimethacrylate.

[0118] After analysis and balance: the average conversion rate of the reaction raw materials is 95.6%, the content of methyl tributylacetonate oxime silane in the product is 95.37%, the extraction rate of the turbo extraction tower product is 85.5%, the yield of methyl tributylacetonate oxime silane in the reaction process is 93.4%, and the purity of the value-added product ammonium chloride is 94.1%.

[0119] <Comparative Example 3>

[0120] A method for extracting methyl tributylidene oxime silane comprises the following steps:

[0121] S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is the butanone oxime hydrochloride precipitate;

[0122] S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower;

[0123] S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling;

[0124] S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters the neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained.

[0125] The feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.48:1.

[0126] The temperature in S1 is 35°C.

[0127] After the reaction in S1, part of the material is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

[0128] The solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

[0129] The feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:2.

[0130] In the extraction tower of S2, multiple turbines are arranged. The turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

[0131] The amount of extraction enhancer added is 0.1% of 120# solvent gasoline.

[0132] The preparation method of the extraction enhancer is:

[0133] 30 kg of 1-aminopropyl-3-methylimidazole nitrate is added to 300 kg of DMF, and after stirring and mixing evenly, 2 kg of triethylamine is added, and then the mixture is stirred and reacted at room temperature for 20 minutes, and then 0.01 kg of acryloxysilane is added, the temperature is controlled at 50° C., and the mixture is stirred and reacted for 20 minutes, and then 12 kg of ethylene glycol acrylate is added, the temperature is controlled at 50° C., and the mixture is stirred and reacted for 120 minutes, and DMF is removed by distillation under reduced pressure to obtain an extraction enhancer.

[0134] The acryloxysilane is selected from 3-(methacryloyloxy)propyltrimethoxysilane (CAS No.: 2530-85-0).

[0135] The ethylene glycol acrylate is selected from ethylene glycol dimethacrylate.

[0136] After analysis and balance: the average conversion rate of the reaction raw materials is 96.5%, the content of methyl tributylacetonate oxime silane in the product is 96.72%, the extraction rate of the turbo extraction tower product is 86.3%, the yield of methyl tributylacetonate oxime silane in the reaction process is 94.2%, and the purity of the value-added product ammonium chloride is 95.0%.

[0137] Although the present invention has been described in detail above by means of general description, specific implementation methods and tests, it is obvious to those skilled in the art that some modifications or improvements may be made to the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection claimed by the present invention.

Claims

1. A method for extracting methyl tributylidene oxime silane, characterized in that: The steps include: S1: methyltrichlorosilane, butanone oxime and 120# solvent gasoline are continuously pumped into a stirred reactor by a feed pump through a flow meter, and the reaction temperature is controlled. After the reaction, the materials are discharged to a two-phase separator for sedimentation and stratification. The upper layer is the solvent and methyltributylacetoximosilane, as well as unreacted butanone oxime and a small amount of crude butanone oxime hydrochloride entrained, and the lower layer is butanone oxime hydrochloride precipitate; S2: After the solvent and unreacted butanone oxime in the upper layer are neutralized with ammonia, the ammonium chloride solid is filtered out, and the solvent and unreacted butanone oxime are evaporated through a thin film evaporator, and the bottom is the methyl tributylidene silane product; the solvent and unreacted butanone oxime evaporated through the thin film evaporator are pumped into the bottom of the turbine extraction tower, and the butanone oxime hydrochloride precipitate in the lower layer is pumped into the top of the turbine extraction tower; S3: The crude solvent and the butanone oxime hydrochloride precipitate are subjected to liquid-liquid mass transfer in a turbine extraction tower, and the extracted solvent containing the methyl tributyone oxime silane product overflows from the top of the extraction tower and is pumped into the reactor in S1 for recycling; S4: The butanone oxime hydrochloride precipitate after extraction is taken out from the bottom of the tower and enters a neutralizer for neutralization reaction with liquid ammonia. After distillation and drying, butanone oxime, a small amount of solvent and ammonium chloride solid can be obtained; An extraction enhancer is also added to the S1, the amount of which is 0.1-1% of 120# solvent gasoline; The preparation method of the extraction enhancer is: According to the mass proportions, 30-50 parts of 1-aminopropyl-3-methylimidazole nitrate and 0.001-0.1 parts of ferric acrylate are added to 300-400 parts of DMF, and after being stirred and mixed evenly, 2-5 parts of triethylamine are added, and then the mixture is stirred and reacted at room temperature for 20-40 minutes, and then 0.01-0.3 parts of acryloxysilane are added, the temperature is controlled at 50-70°C, the mixture is stirred and reacted for 10-20 minutes, and then 12-22 parts of ethylene glycol acrylate are added, the temperature is controlled at 50-70°C, the mixture is stirred and reacted for 100-120 minutes, and DMF is removed by distillation under reduced pressure to obtain an extraction enhancer.

2. The method for extracting methyl tributylidene oxime silane according to claim 1, characterized in that: The feed mass ratio of methyltrichlorosilane, butanone oxime and 120# solvent gasoline in S1 is 1:3.48-3.65:

1.

3. The method for extracting methyl tributylidene oxime silane according to claim 1, characterized in that: The temperature in S1 is 35-45°C.

4. The method for extracting methyl tributylidene oxime silane according to claim 1, characterized in that: After the reaction in S1, part of the material is cooled in a circulating cooler and then circulated to the reactor, and part of the material is taken out and sent to a two-phase separator.

5. The method for extracting methyl tributylidene oxime silane according to claim 1, characterized in that: The solvent and unreacted butanone oxime in S2 are evaporated and collected by an evaporator.

6. The method for extracting methyl tributylidene oxime silane according to claim 1, characterized in that: The feed volume flow ratio of the solvent and the unreacted butanone oxime mixture to the butanone oxime hydrochloride precipitate in S2 is 1:2-3.

7. The method for extracting methyl tributylidene oxime silane according to claim 1, characterized in that: In the extraction tower of S2, multiple turbines are arranged. The turbine stirring drives the turntable to rotate at a high speed to generate pulses, so that the two phases generate driving force in the axial direction, thereby increasing the flooding flow rate of the two phases.

8. The method for extracting methyl tributylidene oxime silane according to claim 1, characterized in that: The acryloxysilane is selected from at least one of 3-(methacryloyloxy)propyltrimethoxysilane and 2-acrylate 3-(diethoxymethylsilyl)propyl ester; the ethylene glycol acrylate is selected from at least one of ethylene glycol dimethacrylate, tetraethylene glycol dimethacrylate and triethylene glycol dimethacrylate.

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