CN1183143C - Industrial process for preparing dialkyldialkoxyl silane - Google Patents
Industrial process for preparing dialkyldialkoxyl silane Download PDFInfo
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Abstract
The present invention relates to an industrial process for preparing dialkyldialkoxyl silane, particularly to a high-yield industrial process for preparing dialkyldialkoxyl silane by directly making alkane halide, magnesium and n-silicate mutually react. The method also comprises post-treatment steps that after materials obtained in reaction are filtered and washed by ether solvents, solvents are rectificated and recovered, target dialkyldialkoxyl silane products are obtained, and filter cakes are successively treated by water and acid to make target products and solvents in the filter cakes recovered.
Description
The present invention relates to a process for the industrial production of dialkyldialkoxysilanes. In particular, the present invention relates to a process for the high-yield commercial production of dialkyldialkoxysilanes directly from the mutual reaction of an alkyl halide, magnesium and an orthosilicate. The method also comprises the post-treatment steps of filtering the material obtained by the reaction, washing the material by an ether solvent, rectifying and recovering the solvent to obtain a target product dialkyl dialkoxy silane, and treating the filter cake by water and acid to recover the target product and the solvent in the filter cake.
The dialkyl dialkoxy silane has important application in the industrial fields of polymer synthesis and the like, such as a structure control agent of organic silicon rubber compound, a stereo modifier of a catalyst in polypropylene production, a room temperature vulcanized silicone rubber chain extender, a synthetic reagent of an organic silicon vinyl end socket and the like, and can be produced by various methods. The disclosed production method mainly comprises an alcoholysis method of alcoholysis reaction of alkyl chlorosilane and methanol; an ester cracking method in which a dialkyl polycyclosiloxane and an orthosilicate ester monomer are subjected to an ester cracking reaction; and a selective alkylation method in which an orthosilicate is reacted in the presence of a Grignard reagent. Among these production methods, the selective alkylation method using Grignard reagents has problems to be solved such as poor process stability, low yield, complicated post-treatment process, environmental pollution caused by organic solvents, etc., and thus has difficulties in practical industrial production,
For example, U.S. patent No. u.s.p4958041, a laboratory method for preparing dialkyldialkoxysilanes is provided by reacting a tetraalkoxysilane or a trialkoxymonosilane with a grignard reagent to prepare the dialkyldialkoxysilane. The workup of the process requires the addition of a small amount of methanol to the reaction mass to convert the excess Grignard reagent into alkoxy organic salts. The filtration becomes easier. This, while effective, adds an auxiliary raw material, and the desired product dialkyldialkoxysilane is severely limited in methanol content. If the loss of the methanol dosage is mastered and the methanol content in the product exceeds the standard, unqualified products can be caused. The post-treatment also comprises the steps of filtering the reaction materials, washing a filter cake by using ethers, combining the filtrate with the washing liquid, and removing the solvent to obtain the target product. Because the dosage of the washing solvent cannot be overlarge and the washing times are limited, the washing effect cannot be very high, a filter cake necessarily contains considerable target products, and the method not only has a complex process, but also causes yield loss.
Japanese patent application laid-open No. 6-345781 provides a laboratory preparation method of dialkyl dialkoxy silane, which has high reaction medium cost and is not suitable for industrial production. The post-treatment of the method is to add an aqueous solution of inorganic salt, add acid to treat the reaction material, dissolve the solid material in the reaction material into inorganic salt and enter a water phase, leave the target product in the reaction material in an organic phase, and remove the solvent from the organic phase to obtain the target product. The method avoids the operations of filtration and corresponding washing of filter cakes. However, the yield of the desired product is low because the loss of the dialkyldialkoxysilane due to hydrolysis is considerable.
The inventor of the invention has intensively studied and finally developed the method of the invention, and the purpose of satisfying the defects of the prior art and producing the dialkyl dialkoxy silane with high efficiency in industrialization is realized.
Therefore, the present invention aims to provide an industrial production method of dialkyldialkoxysilanes, which effectively overcomes the defects of the prior art due to stable process, simplicity, reliability, high yield, low cost and reduced environmental pollution. It is also an object of the present invention to provide a dialkyldialkoxysilane target product produced in this way. Other objects of the invention will become apparent from the further description of the invention.
The invention relates to an industrial production method of dialkyl dialkoxy silane, which comprises the following steps: a. b, adding halogenated alkane and magnesium in an ether solvent in the presence of a catalyst, heating while stirring until reflux occurs, starting the reaction, continuing the reaction for 0.5 to 3 hours, then dropwise adding a mixed solution of the halogenated alkane and orthosilicate ester dissolved in the ether solvent while stirring, continuously refluxing for 4 to 8 hours after the dropwise adding is finished, cooling to room temperature, adding the organic liquid phase material recovered in the previous step d, continuing stirring to enable the temperature of the material to be close to room temperature, c, filtering the reaction material, washing a filter cakeby using the ether solvent, combining a washing solution with the filtrate, and rectifying to recover the ether solvent and the dialkyldialkoxysilane respectively; and d, further soaking the filter cake treated in the step c in water, separating out an upper organic liquid phase, then adding acid for treatment, separating the upper organic liquid phase again, combining the upper organic liquid phase and recovering the organic liquid phase twice, returning the organic liquid phase to the subsequent step b, participating in the filtration, washing and rectification, and further recovering the ether solvent and the dialkyl dialkoxy silane still remained in the organic liquid phase.
The reaction in the process of the invention is as follows:
1.
2.
3.
4.
in the above reaction formula, R1Is alkyl or cycloalkyl, preferably C1-C8Alkyl or C3To C10Cycloalkyl groups such as isopropyl, isobutyl, cyclopentyl: r2Is an alkyl radical, preferably C1-C8Alkyl groups such as methyl; x is halogen, such as chlorine. Accordingly generateInorganic salts of (e.g. MgCl)2. As can be seen from the above reaction scheme, in the process of the present invention, the haloalkane R is first used1X reacts with magnesium Mg in ether solvent in the presence of catalyst to generate R1MgX, and then reacting this intermediate with the subsequent addition of orthosilicate Si (OR)2)4The dialkyl dialkoxyl silane R is prepared by reaction1 2Si(OR2)2. The reaction scheme in set 3 illustrates the main reaction that occurs when the filter cake is treated with water. Set 4, equations 1 and 2 illustrate the main reactions that occur when the filter cake is directly treated with acid. Set 4, reaction formula 3 illustrates the reaction that occurs when the filter cake is first treated with water, and the reaction of set 3 occurs followed by treatment with acid. Adding organic liquid phase material recovered by the previous batch of filter cake treatment into the reaction material, and because the organic phase material contains a small amount of water and acid, the 3 rd group reaction and the 4 th group reaction can simultaneously occur. After the treatment, the organic magnesium salt on the filter cake can be converted into inorganic magnesium salt which is dissolved in water phase, and the target products of dialkyl dialkoxy silane and ether solvent carried on the filter cake are shown as organic phase which is recycled.
The process of the invention is more specifically summarized as follows: the invention provides an industrial production method of dialkyl dialkoxy silane, which comprises the steps of adding magnesium, a catalyst, partial halogenated alkane and an ether solvent into a reaction kettle which is provided with a stirring device, a reflux condenser, a temperature measuring instrument and a liquid material dropping device and can be heated and cooled, heating, refluxing and starting the reaction; under reflux, a solution of the remaining haloalkane, orthosilicate and ether is added dropwise with stirring. After the dripping is finished, the mixture is heated moderately and maintained to reflux for a plurality of hours; then the temperature of the reaction material is reduced to be close to the room temperature, the organic liquid phase material recovered by the previous batch of filter cake is added, and the stirring is continued to ensure that the temperature of the material is keptNear room temperature. The material is filtered in a filter tank, and the filter cake is washed with ether solvent. The obtained filtrate and washing liquor are combined for rectification, and the ether solvent is recovered to obtain the target product. The filter cake is transferred to another device and soaked by water, and the upper layer organic phase liquid material is separated. And adding acid for treatment, and continuously separating out the upper organic phase liquid material. The organic phase liquid materials obtained by water treatment and acid treatment are combined for the next batch of reactionAfter the reaction is finished, adding the mixture into the next batch of reaction materials, and recycling a small amount of water and acid contained in the organic phase liquid material and excessive R in the reaction materials1MgX reacts to generate inorganic salt which is easy to filter, and the target product and ether solvent remained on the filter cake are recovered. The inorganic magnesium salt can be recovered from the water phase solution after water and acid treatment.
The reaction is carried out at 0-100 deg.C, usually at 28 deg.C or higher, and at 40 deg.C or higher, the reaction speed is increased. Preferably, the reaction of the present invention is carried out at reflux temperature at all times after the start of the reaction. Reaction time: step a typically takes from 1.5 to 4 hours; step b takes 6 to 20 hours, which is related to the product type, the charge and the design of the reactor. As can be readily determined by one of ordinary skill in theart.
The ether solvent suitable for use in the present invention may include any ether conventionally used in the art, preferably methyl t-butyl ether.
The catalyst suitable for the present invention is iodine, which is used in an amount of 0.01% to 1% based on the total weight of the reaction system.
Although halogenated alkanes conventionally used in the art can be used, a suitable halogenated alkane is preferably a chlorinated alkane such as chloroisopropane or the like, in view of the economical efficiency of industrial production.
The raw material of the invention is divided into two parts. As described above, a part of the raw materials was charged into the reaction vessel as "bottom material", and the rest of the raw materials were charged as "dropping material", and then dropped into the reaction vessel after the start of the reaction. The invention pays attention to the dosage of halogenated alkane in the bottom material in order to ensure that the reaction is smoothly and stably started, and obtains satisfactory effect in the industrial production of target products. The halogenated alkane in the "primer" accounts for 10 to 25 percent, preferably 12 to 16 percent of the total weight of the halogenated alkane feed. The ether solvent in the bottom material accounts for 10-40 wt%, preferably 15-25 wt% of the total ether solvent.
The feeding molar ratio of the invention is 1: 2 to 1: 4, preferably 1: 2.2 to 1: 3 based on the orthosilicate; the molar ratio of orthosilicate to magnesium is 1: 2 to 1: 3, preferably 1: 2.2 to 1: 2.7; the molar ratio of the orthosilicate to the catalyst is from 1: 0.0001 to 1: 0.0004, preferably from 1: 0.0002 to 1: 0.0003; the molar ratio of orthosilicate to ether is from 1: 3 to 1: 10, preferably from 1: 5 to 1: 9.
A small excess of R is present in the reaction mass obtained according to the invention1The MgX residue is not converted into alkoxy magnesium salt by using methanol for treatment as in the prior art U.S. P4958041, but is converted into inorganic magnesium salt by using a small amount of water and acid contained in an organic phase material recovered by treating a filter cake, so that the MgX residue is not only cheap and effective, but also meets the requirements of high efficiency and low consumption in industrial production, and is beneficial to realizing industrial production.
The post-reaction treatment of the invention is as described above, the reaction material is added with the filter cake of the previous batch to recover the liquid material of the organic phase, then the filtration is carried out, the filter cake is washed by ether solvent, the filtrate and the washing liquid are combined and rectified to obtain the target product, and the solvent is recovered. Soaking the filter cake in water, recovering the organic phase layer, and then pickling to recover the organic liquid phase layer. The inorganic magnesium salt can be recovered from the water phase. The post-treatment process solves the problems that the recovery rate of the product is difficult to improve because the pure filtration washing operation is limited by the dosage and the frequency of the washing agent, so that the product and the solvent remained on the filter cake are recovered, and the product yield is improved to a greater extent. And simultaneously, the problems that the reaction is violent when materials are treated by acid only, the filtering and washing operation is avoided, the product hydrolysis loss is large, and the yield of the target product of the dialkyl dialkoxy silane is difficult to improve are solved. The operation of the water treatment material is the characteristic of the invention. It has the advantages that: mild conditions and small hydrolysis loss of the product. However, the interface is not obvious because an oil-water transition layer is arranged between the organic phase and the aqueous phase. So the filter cake is soaked in water, the organic phase material on the upper layer is removed, then the oil-water transition layer is treated by acid, and the small part of the organic phase material is obtained by continuous separation. The treatment reduces the hydrolysis loss of the target product remained on the filter cake to the maximum extent, improves the recovery rate of the product, and ensures that the water consumption for soaking the filter cake is 3 to 6 times of the weight of the filter cake. The acid used is an inorganic acid, such as hydrochloric acid. The acid is used in an amount to make the water phase slightly acidic at last, and the pH value is 3-6.5.
The reaction kettle used in the invention is a stainless steel reaction kettle which is preferred in order to meet the heat transfer requirement, and is also applicable to a glass lining reaction kettle. But not limited to reactors of other materials.
The invention is further illustrated by the following examples which are intended to be illustrative only and are not intended to be in any way limiting to the scope of the invention.
Example 1
36.8kg of magnesium chips (purity 99%, 1.5Kmol), 19.0kg of chloroisopropane (purity 99%, 0.24Kmol), 65.0kg of methyl tert-butyl ether (purity 98%, 0.74Kmol) and 10g of iodine are put into a 1000L stainless steel reaction kettle provided with an electric stirring device, a reflux condenser, a thermometer and a liquid dropping device, electric heating is started, the temperature of the kettle rises, reflux occurs, and the reaction starts. When the reflux was reduced, stirring was started and a solution of 100.0kg (purity 99%, 1.26kmol) of chloroisopropane, 94.5kg (purity 99%, 0.615kmol) of methyl orthosilicateand 200.0kg (purity 98%, 2.22kmol) of methyl tert-butyl ether in the dropping pot was dropped into the reaction vessel. After the materials are dripped, the reflux reaction is continued for 5 hours, the temperature is reduced, the sampling analysis is carried out, the conversion rate of the methyl orthosilicate is 100 percent, the reaction materials are put into a filter tank, the vacuum filtration is carried out, 360kg of methyl tert-butyl ether (with the purity of 98 percent and the purity of 4.0kmol) is used for washing for four times, then a filter cake is soaked by water, and 66.0kg of organic phase liquid materials are separated.
And feeding and producing according to the scheme. The conversion rate of the methyl orthosilicate is 100 percent, and 74.0kg of organic phase liquid material is separated by soaking a filter cake in water.
The filtrate and the washing liquid produced in the two batches are combined and rectified to obtain 179kg of diisopropyldimethoxysilane product with the purity of 99.35 percent and the yield of 82 percent, and the organic phase liquid material can be recovered by soaking and separating the two batches of filter cakes with water, so that the yield can be improved by 12.8 percent. The total yield is 94.8%.
Example 2
The process was carried out as in example 1. After the reaction, samples were taken for analysis. The conversion rate of the methyl orthosilicate is 100 percent. The reaction mass is put into a filter tank, and the operations of filtering and washing are carried out by the same method. Then the filter cake is removed and soaked by water, 39kg of organic phase liquid is obtained by coarse separation, and the gas chromatographic analysis shows that the filter cake contains 16.98 percent of diisopropyl dimethoxy silane. Roughly separating the material after the organic phase liquid material is transferred out, adding hydrochloric acid for treatment, measuring the pH value of an aqueous phase to be 6, standing for layering, separating to obtain 20kg of organic phase liquid material, and analyzing by gas chromatography to obtain 22.81% of diisopropyl dimethoxy silane. 11.2kg of diisopropyl dimethoxysilane can be recovered from the organic phase liquid obtained by water treatment and acid treatment, and the yield is improved by 10.3 percent.
Example 3
The example is a laboratory preparation method of diisopropyl dimethoxysilane, which plays a guiding role in establishing the industrial production method of the product:
24.5g of magnesium chips (with the purity of 99 percent and the purity of 1.0mol), 12.8g of chloroisopropyl (with the purity of 99 percent and the purity of 0.16mol), 40ml of methyl tert-butyl ether (with the purity of 30g and the purity of 0.34mol) and 0.1g of iodine are put into a 500ml reaction bottle provided with a thermometer, a magnetic stirring device and a reflux condenser, stirring is started, electric heating is started, the temperature of reaction materials is raised, reflux is generated, and the reaction is started. A solution prepared from 62.8g of methyl orthosilicate (99% pure, 0.41mol), 66.6g of chloroisopropane (99% pure, 0.84mol) and 200ml of methyl tert-butyl ether (150g, 1.7mol) was added dropwise. During the dropping process, the reflux state is maintained by electric heating. After the dropwise addition, the reaction was carried out for 6 hours while maintaining the reflux state, and the temperature was lowered, sampled and analyzed. The conversion rate of methyl orthosilicate is 99.7%. The filter cake was filtered and washed four times with 200g of methyl tert-butyl ether. The filtrate and the washing liquid are combined and rectified. 66.4g of diisopropyldimethoxysilane was recovered in 92% yield.
The experiment was repeated 7 times under this process condition. The reaction can be smoothly and stably started in each experiment, the conversion rate of the methyl orthosilicate is close to 100%, and the product yield is 90-96%.
Comparative example 1
Validation experiments were performed according to the laboratory preparation of diisopropyldimethoxysilane as provided in example 6 of U.S. p4958041:
24.5g of magnesium chips (purity 99%, 1.0mol), 3.2g of chloroisopropane (purity 99%, 0.04mol), 20ml of methyl t-butyl ether (15g, 0.17mol) and 0.1g of iodine were charged into a 500ml reaction flask equipped with a thermometer, a magnetic stirrer, a dropping liquid device and a reflux condenser. Stirring was started, electric heating was started to raise the temperature of the reaction mass to generate reflux, and a solution prepared from 62.8g of methyl orthosilicate (purity 99%, 0.41mol), 76.2g of chloroisopropane (purity 99%, 0.96mol) and 140ml of methyl tert-butyl ether (104g, 1.18mol) was added dropwise. During the dropping process, the reflux state is maintained by electric heating. After the completion of the dropwise addition, the reflux state was maintained for 6 hours. Magnesium chips were observed to be still present in large amounts. The reflux reaction was continued for 46 hours, and a sample of the reaction solution was taken for gas chromatography analysis, and 16.5% of the methyl orthosilicate was still unconverted.
Comparative example 2
Japanese Kokai Hei-6-34578 example 7 describes a laboratory preparation of diisopropyldimethoxysilane:
a Grignard reagent isopropyl magnesium chloride was prepared by charging 26.7g of magnesium metal (1.1 g molecular) into a 2 liter flask equipped with a stirrer, a reflux condenser, a thermometer, and a dropping funnel, further charging 300ml of tetrahydrofuran and a small amount of iodine, adjusting the internal temperature to 40 to 50 ℃ under nitrogen atmosphere, adding 86.4g of isopropyl chloride (1.1 g molecular) dropwise within 1 hour, and further stirring at 55 ℃ for 1 hour. To the reaction solution was added 300ml of toluene, and then 76.1g of methyl orthosilicate (0.5 g molecule) was added dropwise over 1 hour at room temperature through a dropping funnel, and 300ml of a 10% ammonium chloride aqueous solution was added from the dropping funnel and stirred. Then, 182.0g of 20% hydrochloric acid (1.0 mol) was added to the lower aqueous phase with a pump under gentle stirring over 1 hour to dissolve the by-produced salts. Then, the stirring was stopped, and the reaction solution was subjected to a liquid separation operation to remove the aqueous phase. When the organic phase was distilled, unhindered distillation was achieved and 70.5g of diisopropyldimethoxysilane was obtained. The yield thereof was found to be 80%.
Example 4
29.5kg of magnesium chips (purity 99%, 1.2mol), 25.0kg of chlorocyclopentane (purity 99%, 0.24kmol), 70.0kg of methyl tert-butyl ether (purity 98%, 0.78kmol) and 15g of iodine are put into a 1000L glass lining reaction kettle provided with an electric stirring device, a reflux condenser, a thermometer and a liquid dropping device, a steam valve is opened, and the materials are heated by a jacket to be heated. Reflux occurred and the reaction started. After 1 hour, a solution of 101.8kg (purity 99%, 0,96kmol) of chlorocyclopentane, 77.2kg (purity 97%, 0.49mol) of methyl orthosilicate and 120.0kg (purity 98%, 1.334kmol) of methyl tert-butyl ether in the addition tank was added dropwise into the reaction vessel. After the dropwise addition of the materials, the reaction was continued under heating and reflux for 6 hours. And (5) cooling, sampling and analyzing. The conversion rate of the methyl orthosilicate is 100 percent. And (3) putting the reaction materials into a filter tank, and performing vacuum filtration. Further, the residue was washed with 280.0kg of methyl t-butyl ether (purity: 98%, 3.113 kmol). The filter cake was treated with hydrochloric acid to obtain 14kg of organic phase liquid. The filtrate and the washing liquid are combined and rectified to obtain 91.5kg of dicyclopentyldimethoxysilane with the purity of 99.8 percent. 10.4kg of dicyclopentyldimethoxysilane can be recovered by filter cake treatment of liquid material of the organic phase and other rectification fractions. The total yield is 90.6%.
Example 5
36.8kg (purity 99%, 1.5kmol), 20.0kg (purity 98%, 0.212kmol) of chloroisobutane, 65.0kg (purity 98%, 0.74kmol) of methyl tert-butyl ether and 15g of iodine are put into a 1000L stainless steel reaction kettle provided with an electric stirring device, a reflux condenser, a thermometer and a liquid material dropping device, electric heating is started, the temperature of the kettle rises, reflux occurs, and the reaction is started. When the reflux is weakened, stirring is started, and a solution formed by 121.7kg (purity 98 percent, 1.288kmol) of chloroisobutane, 95.5kg (purity 98 percent, 0.615kmol) of methyl orthosilicate and 180kg (purity 98 percent, 2.0kmol) of methyl tert-butyl ether in the dropping tank is dropped into the reaction kettle. After the addition of the material, the reaction was continued under reflux for 6 hours. And (5) cooling, sampling and analyzing. 116.6kg of diisobutyldimethoxysilane was produced.
The production is carried out again according to the scheme to generate 118.3kg of diisobutyldimethoxysilane.
The materials obtained from the two batches of reactions are directly put into a filter tank for filtration, and 360kg of methyl tert-butyl ether is respectively used for washing filter cakes. And combining the two batches of filtrate and washing liquor for rectification to obtain 124kg of diisobutyldimethoxysilane with the purity of 98.6 percent. 54.2kg of diisobutyldimethoxysilane product can be recovered from other fractions. 176.5kg of diisobutyldimethoxysilane was produced in total, 70.3% yield relative to the theoretical yield and 75.1% yield relative to the actual amount of reaction. Neglecting the rectification losses, it can be considered that the filtration wash recovery is about 75% and the product loss remaining on the filter cake accounts for 25% of the actual production.
Example 6
The batch and process operation were carried out as in example 5. After the reaction, samples were taken for analysis. 114.9kg of diisobutyldimethoxysilane was produced. The reaction mass was filtered directly and the filter cake was washed several times with 360kg of methyl tert-butyl ether. The filtrate and the washing liquid are combined for rectification. And adding 3 times of water into the filter cake for soaking to obtain slurry liquid, and adding a small amount of hydrochloric acid for multiple times to finally obtain the pH value of the water phase of 5-6. Standing, separating to obtain 54.0kg of organic phase liquid material, and carrying out chromatographic analysis to recover 17.1kg of diisobutyldimethoxysilane, wherein the theoretical yield is improved by 13.6 percent (relative to the theoretical yield) and the actual yield is improved by 14.9 percent (relative to the actual yield of the reaction).
Claims (13)
1. An industrial production method of dialkyl dialkoxyl silane is characterized by comprising the following steps: a. b, adding a mixed solution of halogenated alkane and ortho-silicate dissolved in an ether solvent while stirring, heating until reflux occurs, reacting for 0.5 to 3 hours, then dropwise adding the mixed solution of the halogenated alkane and the ortho-silicate dissolved in the ether solvent whilestirring, continuously refluxing for 4 to 8 hours, cooling to room temperature, adding the organic liquid phase material recovered in the previous step d, continuing stirring to enable the temperature of the material to be close to the room temperature, c, filtering the reaction material, washing a filter cake with the ether solvent, combining a washing solution with a filtrate, and rectifying to recover the ether solvent and the dialkyl dialkoxy silane respectively; and d, further soaking the filter cake treated in the step c in water, separating out an upper organic liquid phase, then adding acid for treatment, separating the upper organic liquid phase again, combining the upper organic liquid phase and recovering the organic liquid phase twice, and returning the organic liquid phase to the subsequent step b.
2. The process according to claim 1, wherein the reaction temperature in steps a and b, which are the same or different, is 0 to 100 ℃.
3. The process according to claim 1, wherein the amount of haloalkane used in step a is 10 to 25% by weight based on the total amount of haloalkane used in steps a and b.
4. The process according to claim 1, characterized in that the molar ratio of orthosilicate to haloalkane in the reaction system is from 1: 2 to 1: 4; the mol ratio of the orthosilicate ester to the magnesium is 1: 2-1: 3; the mol ratio of the orthosilicate and the catalyst is 1: 0.0001-1: 0.0004; and the mol ratio of the orthosilicate ester to the ether solvent is 1: 3-1: 10.
5. A process according to claim 1, characterised in that the dialkyldialkoxysilane has the formula R1 2Si(OR2)2In the formula, R1Is alkyl or cycloalkyl; r2Is an alkyl group.
6. A process according to claim 5, characterized in that R is1Represents isopropyl, isobutyl or cyclopentyl; and R2Represents a methyl group.
7. The process according to claim 1, wherein the halogenated alkane is chloroisopropane, oxoisobutane, chlorocyclopentane, etc.
8. The method according to claim 1, characterized in that the orthosilicate is methyl orthosilicate.
9. The process according to claim 1, wherein the ethereal solvent is methyl tert-butyl ether.
10. The process of claim 1 wherein the catalyst is iodine.
11. The method of claim 1, wherein the filter cake after filtration and washing is soaked with water in an amount of 3-6 times the weight of the filter cake to separate an organic phase liquid material; then acid treatment is carried out to make the water phase become slightly acidic, and the organic phase liquid material is separated again.
12. The method of claim 1, wherein the filtered, washed filter cake is soaked in water with an acid added in an amount to make the aqueous phase finally acidic.
13. A process according to any one of claims 1, 11 or 12, characterised in that the acid is hydrochloric acid.
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