CN104151346A - Method for producing dimethyl cyclosiloxane in non-halogenation direct continuous mode - Google Patents
Method for producing dimethyl cyclosiloxane in non-halogenation direct continuous mode Download PDFInfo
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Abstract
The invention relates to a method for producing dimethyl cyclosiloxane in a non-halogenation direct continuous mode. The method comprises the following steps: firstly, performing pretreatment and activation treatment on silicon powder, putting into a reaction kettle together with a solvent, sealing the reaction kettle, heating, feeding a certain amount of methyl bromide, subsequently continuously feeding dimethyl ether into the reaction kettle for performing non-halogenation direct synthesis reaction, separating the mixture generated in the reaction into a high melting point material and a low melting point material through a separation column, returning the high melting point material, circulating into a reactor again, further condensing the low melting point material, and feeding methylsiloxane condensate in the low melting point material into a distillation device for separating dimethyl cyclosiloxane (DMC). In the whole process, significant indexes such as the selection rate of DMC and the components of unreacted mixed gases are monitored on line by using a gas chromatographic method, and basis is provided for continuous on-line control. By adopting the method, continuous production and automatic process control can be achieved in the dimethyl cyclosiloxane preparation process, and thus purposes of improving the efficiency, improving the product stability and the like can be achieved.
Description
Technical field
The present invention relates to the production technical field of silicone intermediate, be specifically related to a kind of method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization.
Background technology
The kind of current high performance new chemical materials-organosilicon material has exceeded 10000 kinds, can with product just have more than 5000 kinds, mainly comprise high temperature silicon rubber, room temperature silicon rubber, silicone oil and secondary processing product, silicone resin and silane coupling agent etc.High temperature silicon rubber is widely used in aviation and aerospace industry, automotive industry, electronic apparatus; Room temperature silicon rubber is for building industry, electronic industry, road construction, as materials such as sealing, bonding perfusion, coatings; Silicone resin is because of its splendid thermotolerance, and good electrical insulating property, chemical-resistant resistance and hydrophobic nature, flame retardant resistance, mainly as heat resistant varnish, high-temperature resistant coating, tackiness agent, weather-resistant coating and hydrophobic coating.Organosilicon material development in recent years rapidly, except Asian market keeps the annual growth of 12%-15%, the organosilicon market that the U.S. and West Europe etc. are the most ripe, its tempo, also higher than the growth of its GDP, reaches 4%～6%, global amplification maximum be China, exceed 25%, within 2009, Chinese organosilicon material consumption just exceedes 400,000 tons, and exceeding the U.S. becomes the maximum country of consumption of organosilicon material, accounts for 30% of global consumption.At present the organosilicon material output in the whole world exceedes 1,350,000 tons, most developed countries all using organosilicon material as 21 century novel material emphasis developed.
Estimate that in a few years from now on, the average growth rate per annum of global organosilicon demand is about 6%, the average growth rate per annum of China's organosilicon consumption will keep 20% left and right.Along with the fast development of the industry such as the electric industry of recent year, building and automotive industry, textile printing and dyeing, silicone industry in China product consumption sharply increases, the industry pillar of organosilicon industry is the production of the polysiloxane of basis, upstream intermediate raw material-Primary Speciation, and domestic production capacity deficiency causes all needing every year the silicone monomers product of a large amount of import Primary Speciations.In these products, more than 90% be dimethyl cyclosiloxane (being called for short DMC), DMC really can be directly used in the synthetic main raw material of downstream fine product in organosilicon industry, be also the source of profit that organosilane monomer corporate boss wants simultaneously.It is predicted, after 2014, domestic monomer export volume can increase gradually, and the DMC of high added value and portion downstream product thereof will have wide market outlook.Therefore, DMC synthetic technology level height directly affects the ups and downs of organosilicon industry, and countries in the world all give special concern.
The forties in last century, Rochow has invented the direct technology of preparing of Halogen of DMC, and this technology has that raw material is easy to get, solvent-free, space-time yield is high, easily realize the advantages such as serialization production, once appearance, develops rapidly and becomes the main flow of DMC production technology.
The direct preparation technology of DMC Halogen is: taking Pure Silicon Metal and methyl chloride as raw material, copper is catalyzer, and direct reaction generates methyl chlorosilane mix monomer.Synthetic mix monomer, through high precision rectification, is isolated a series of methyl chlorosilane monomers, and wherein dimethyldichlorosilane(DMCS) accounts for the 80-93% of total amount.The further hydrolysis of this product, cracking, rectifying can be prepared DMC.And the by product HCl of the methyl chlorosilane monomer hydrolysis recovery of purifying, making methyl chloride synthesizes for monomer again, has formed the cycle applications of chlorine element in each workshop section in whole technical process.Above-mentioned technological process is simple to be represented as shown in Figure 3.
Although the direct technology of preparing advantages of above-mentioned DMC Halogen, industrial application is extensive.But also there is long flow path, complex process equipment, the drawbacks such as production control difficulty.Simultaneously the recycling of chlorine element (cyclic utilization rate is 70%-80% only) in production process, not only increases expense, and causes a large amount of HCl to produce, etching apparatus, contaminate environment.Therefore in this sustained economic development, energy growing tension, day by day serious epoch of pollution, the green synthetic replacement technology of development DMC is extremely urgent.
Current research is found, adopts metallic silicon power and dme, taking copper as catalyzer, under non-halogen condition, can prepare DMC by single step reaction.The intrinsic drawback that this technique has not only avoided chlorine element to recycle in above-mentioned traditional technology, and process and equipment simple, control easily, therefore there is significant technical advance and prospects for commercial application, and will start new era of DMC green synthesis techniques.DMC Halogen direct method technological invention people Rochow also once foretold: " non-halogenated direct method is prepared with organic siloxane, will be the most challenging work in future ".
In addition, traditional DMC technology of preparing has all adopted intermittent mode to produce, and the inherent characteristics of interrupter method brings inefficiency and the unsettled drawback of product batches in dimethyl cyclosiloxane preparation process, and cannot realize automatic control, thereby increase cost of labor, reduces scale and benefit.
Summary of the invention
A kind of method that provides non-halogenated direct serialization to produce dimethyl cyclosiloxane is provided problem to be solved by this invention, the method can realize serialization production in the preparation process of dimethyl cyclosiloxane and process is controlled automatically, thereby reaches the object of raising the efficiency, increase product stability.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: a kind of method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization, it is characterized in that, and comprise the steps:
(1) dme, monobromethane are derived and entered reactor by pipeline from dme storage tank, monobromethane storage tank respectively, wherein, be provided with molecule screen casing to remove the minor amount of water in dme, monobromethane at this pipeline;
(2) in addition by catalyst mixture and the SiO that removes silicon powder surface layer
2silica flour, fully mix postactivatedly according to weight ratio 1～5:100, import to silica flour/catalyst/solvent storage tank,
(3) after the activation silica flour of the importing in solvent and step (2) is fully mixed according to weight ratio 1～5:1, add together in reactor, airtight, pressure is 0.1～0.3MPa, be warming up to 250 DEG C～320 DEG C, pass into the monobromethane in step (1), the weight ratio of monobromethane and activation silica flour is 0.05～0.15:1, then in reactor, pass into dme continuous measurement, the intake velocity of dme is 10～15 kgs/hr, stirring velocity is 50～100 revs/min, carries out continuous reaction;
(4) mixture that reaction generates is separated and is obtained high boiler material and lower boiling material by separator column, high boiler material passes back into reactor, lower boiling material needs further condensation, wherein the methylsiloxane mixture phlegma in lower boiling material enters the first distillation tower successively, the first condenser enters in still kettle and separates and obtain dimethyl cyclosiloxane, in lower boiling material, the complete dme of unreacted and the monobromethane that do not consume further pass through second column, the second condenser compression is collected, collect respectively incomplete product through different fractions reception storage tank and be again cycled to used in successive reaction.
Preferably, the silica flour of described step (2) is removed the SiO of silicon powder surface layer
2for, take hydrofluoric acid solution and silica flour that weight ratio is 4～6:1, at room temperature stir 0.5～1.5 hour, filter, fully to wash with dehydrated alcohol, vacuum-drying 2～8 hours at 60～90 DEG C, removes the SiO of silicon powder surface layer
2for subsequent use, and silica flour size is 50～250 μ m.
Preferably, the silica flour activation treatment of described step (2) is cryogenic vacuum pre-treatment or Microwave Pretreatment, cryogenic vacuum pre-treatment is to add in crucible after silica flour and catalyzer are fully ground according to weight ratio 1～5:100, be placed in vacuum drying oven, vacuumize, rising temperature to 80～140 DEG C, are incubated 1～6 hour; Microwave Pretreatment is to add in crucible after silica flour and catalyst mixture are fully ground according to weight ratio 1～5:100, is inserted in microwave oven, and the power of microwave oven is 800-1500W, and the time of microwave treatment is 1～5 minute.
Preferably, described activation treatment is cryogenic vacuum pre-treatment or Microwave Pretreatment, cryogenic vacuum pre-treatment is to add in crucible after silica flour and catalyzer are fully ground according to weight ratio 1～5:100, be placed in vacuum drying oven, vacuumize, rising temperature to 80～140 DEG C, are incubated 1～6 hour; Microwave Pretreatment is to add in crucible after silica flour and catalyst mixture are fully ground according to weight ratio 1～5:100, is inserted in microwave oven, and the power of microwave oven is 800-1500W, and the time of microwave treatment is 1～5 minute.
Preferably, the catalyst mixture in the activation treatment of described step (2) is made up of catalyzer and promotor, and catalyzer is neutralized verdigris, copper hydroxide, in cuprous chloride a kind of or more than one; Promotor is zinc oxide or tin or its combination, and the weight ratio of catalyzer and promotor is 50:1～3.
Preferably, the solvent in the synthesis step of described dimethyl cyclosiloxane is paraffin oil, dodecylbenzene, two undecyl benzene etc. a kind of or more than one.
Preferably, the weight ratio of the solvent/silica flour in the synthesis step of described dimethyl cyclosiloxane is preferably 1～5:1.
Preferably, the temperature in the synthesis step of described dimethyl cyclosiloxane is preferably 260 DEG C～300 DEG C.
After reacting completely, carry out the quantitative analysis of selectivity of product by vapor-phase chromatography, calculate the selectivity of DMC; Filtering reacting liquid body obtains solid residue, and washing is dry, the remaining solid masses of weighing, the transformation efficiency of calculating silica flour and dme, the yield of DMC product.With the transformation efficiency of silica flour and dme, the selectivity of DMC and yield are evaluated the quality of synthetic technological condition.
1. the amount (mmol) × 100% of silica flour in the amount (mmol) of silica flour/input reactor in the transformation efficiency of silica flour=siliceous reaction product.
2. the amount (mmol) × 100% of dme in the amount (mmol) of dme/input reactor in the transformation efficiency of dme=siliceous reaction product.
3. the amount (mmol) × 100% of amount (the mmol)/siliceous reaction product of selectivity=generation cyclosiloxane of DMC.
4. the amount (mmol) × 100% of silica flour in the amount (mmol) of yield=generation cyclosiloxane of DMC/input reactor.
The method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization of the present invention, the method is first silica flour to be carried out after pre-treatment and activation treatment, add together with solvent in reactor, airtight, heat up, be raised to after specified temperature, pass into a certain amount of monobromethane, then in reactor, pass into dme continuous measurement, carry out the direct building-up reactions of non-halogenated method, the mixture that reaction generates is separated into high boiler material and lower boiling material by separator column again, high boiler material again circulates and enters reactor after refluxing, lower boiling material needs further condensation, wherein the methylsiloxane phlegma in lower boiling material enters rectifier unit and isolates dimethyl cyclosiloxane (DMC), in lower boiling material, the complete dme of unreacted and the monobromethane that do not consume further compress collection, again be cycled to used in continuous reaction.After successive reaction certain hour, when the key indexs such as the transformation efficiency of the selection rate of DMC, silica flour and dme reach respectively more than 80%, 90% and 95%, stopped reaction, reclaims solvent, finally prepares dimethyl cyclosiloxane product.The key index such as selection rate, the composition of unreacted mixed gas of vapor-phase chromatography on-line monitoring DMC for whole process, for continuous on-line Control provides foundation.The method can realize serialization production in the preparation process of dimethyl cyclosiloxane, process is controlled automatically, raises the efficiency, increases the objects such as product stability thereby reach.
Brief description of the drawings
Below in conjunction with drawings and Examples, the invention will be further described:
Fig. 1 is the process flow sheet that continuous processing is produced dimethyl cyclosiloxane.
1 is silica flour/catalyst/solvent storage tank; 2 is dme storage tank; 3 is monobromethane storage tank; 4 is reactor; 5 is the useless material storage tank of reaction; 6 is that the first distillation tower, 11 is second column; 7 is that the first condenser, 12 is the second condenser; 8 is that unreacted gaseous state raw material is collected storage tank; 9-1 is the first online gas-chromatography, and 9-2 is the second online gas-chromatography; 10 is still kettle; 13-1 is that the first cut receives storage tank, and 13-2 is that the second cut receives storage tank, and 13-3 is that the 3rd cut receives storage tank, and 13-4 is that the 4th cut receives storage tank.
Fig. 2 is that the selection rate of DMC is with the change curve in reaction times.
Fig. 3 is the direct preparation technology of DMC Halogen of prior art.
Embodiment
Below in conjunction with specific embodiment, such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for the present invention is described.The implementation condition adopting in embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in normal experiment.
Describe the present invention in detail below in conjunction with embodiment, should be appreciated that described herein giving an example only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
The pre-treatment of raw material: the dry pre-treatment of dme and monobromethane, in the exit passageway of dme and monobromethane storage tank, add a segment molecule screen casing before entering reactor, remove contained minor amount of water in dme and monobromethane raw material; The pre-treatment of silica flour, takes hydrofluoric acid solution that weight ratio is 5:1 and the silica flour of 150 μ m, at room temperature stirs 1 hour, filters, and fully washs with dehydrated alcohol, and vacuum-drying 5 hours at 80 DEG C, removes the SiO of silicon powder surface layer
2, for subsequent use;
The activation treatment of silica flour: after CuCl, ZnO and Sn are mixed according to weight ratio 50:1:1, obtain catalyst mixture, this catalyst mixture and above-mentioned silica flour are fully mixed according to weight ratio 2:100, mixture is processed 3 minutes with microwave oven, obtains activating silica flour again;
Dimethyl cyclosiloxane synthetic and separating: after dodecylbenzene and above-mentioned activation silica flour are fully mixed according to weight ratio 2:1, add together in reactor, airtight, the pressure in reactor is 0.2MPa, is warming up to 280 DEG C, pass into monobromethane, the weight ratio that ensures monobromethane and above-mentioned activation silica flour is 0.1:1, then in reactor, passes into dme continuous measurement, and the intake velocity of dme is 13 kgs/hr, stirring velocity is 80 revs/min, carries out continuous reaction; The mixture that reaction generates is separated and is obtained high boiler material and lower boiling material by separator column, high boiler material passes back into reactor, lower boiling material needs further condensation, wherein the methylsiloxane mixture phlegma in lower boiling material enters after rectifier unit separates and obtains dimethyl cyclosiloxane, in lower boiling material the complete dme of unreacted and the monobromethane that do not consume further compression collect, be again cycled to used in successive reaction; After successive reaction 10 hours, the selection rate of dimethyl cyclosiloxane, after the transformation efficiency of silica flour and dme acquires a certain degree, stopped reaction, reclaims solvent, finally prepares dimethyl cyclosiloxane product.
Fig. 1 is the process flow sheet that dimethyl cyclosiloxane is produced in non-halogenated direct serialization, Fig. 2 be adopt vapor-phase chromatography detect online DMC moment selection rate with the change curve in reaction times.
After reaction finishes, in conjunction with on-line determination, calculating can obtain the selection rate of reaction product DMC, and silica flour and dimethyl ether conversion rate, as follows:
Embodiment 2:
The pre-treatment of raw material: the dry pre-treatment of dme and monobromethane, in the exit passageway of dme and monobromethane storage tank, add a segment molecule screen casing before entering reactor, remove contained minor amount of water in dme and monobromethane raw material; The pre-treatment of silica flour, takes hydrofluoric acid solution that weight ratio is 5:1 and the silica flour of 120 μ m, at room temperature stirs 1 hour, filters, and fully washs with dehydrated alcohol, and vacuum-drying 5 hours at 80 DEG C, removes the SiO of silicon powder surface layer
2, for subsequent use;
The activation treatment of silica flour: after CuCl and ZnO are mixed according to weight ratio 50:1, obtain catalyst mixture, this catalyst mixture and above-mentioned silica flour are fully mixed according to weight ratio 2:100, mixture, through 120 DEG C of vacuum sinterings 3 hours, obtains activating silica flour again;
Dimethyl cyclosiloxane synthetic and separating: after dodecylbenzene and above-mentioned activation silica flour are fully mixed according to weight ratio 2:1, add together in reactor, airtight, pressure is 0.2MPa, is warming up to 300 DEG C, pass into monobromethane, the weight ratio that ensures monobromethane and above-mentioned activation silica flour is 0.15:1, then in reactor, passes into dme continuous measurement, and the intake velocity of dme is 10 kgs/hr, stirring velocity is 100 revs/min, carries out continuous reaction; The mixture that reaction generates is separated and is obtained high boiler material and lower boiling material by separator column, high boiler material passes back into reactor, lower boiling material needs further condensation, wherein the methylsiloxane mixture phlegma in lower boiling material enters after rectifier unit separates and obtains dimethyl cyclosiloxane, in lower boiling material the complete dme of unreacted and the monobromethane that do not consume further compression collect, be again cycled to used in successive reaction; After successive reaction 12 hours, the selection rate of dimethyl cyclosiloxane, after the transformation efficiency of silica flour and dme acquires a certain degree, stopped reaction, reclaims solvent, finally prepares dimethyl cyclosiloxane product.
After reaction finishes, in conjunction with on-line determination, calculating can obtain the selection rate of reaction product DMC, and silica flour and dimethyl ether conversion rate, as follows:
Embodiment 3:
The pre-treatment of raw material: the dry pre-treatment of dme and monobromethane, in the exit passageway of dme and monobromethane storage tank, add a segment molecule screen casing before entering reactor, remove contained minor amount of water in dme and monobromethane raw material; The pre-treatment of silica flour, takes hydrofluoric acid solution that weight ratio is 5:1 and the silica flour of 200 μ m, at room temperature stirs 1.5 hours, filters, and fully washs with dehydrated alcohol, and vacuum-drying 5 hours at 80 DEG C, removes the SiO of silicon powder surface layer
2, for subsequent use;
Activation treatment: after CuCl and Sn are mixed according to weight ratio 50:1, obtain catalyst mixture, then this catalyst mixture and above-mentioned silica flour are fully mixed according to weight ratio 2:100, microwave oven is processed 5 minutes for mixture, obtains activating silica flour;
Dimethyl cyclosiloxane synthetic: after dodecylbenzene and above-mentioned activation silica flour are fully mixed according to weight ratio 2:1, add together in reactor, airtight, pressure is 0.2MPa, is warming up to 280 DEG C, pass into a certain amount of monobromethane, the weight ratio of monobromethane and above-mentioned activation silica flour is 0.15:1, then in reactor, passes into dme continuous measurement, and the intake velocity of dme is 15 kgs/hr, stirring velocity is 60 revs/min, carries out continuous reaction; The mixture that reaction generates is separated and is obtained high boiler material and lower boiling material by separator column, high boiler material passes back into reactor, lower boiling material needs further condensation, wherein the methylsiloxane mixture phlegma in lower boiling material enters after rectifier unit separates and obtains dimethyl cyclosiloxane, in lower boiling material the complete dme of unreacted and the monobromethane that do not consume further compression collect, be again cycled to used in successive reaction; After successive reaction 8 hours, the selection rate of dimethyl cyclosiloxane reaches 83.4%, and the transformation efficiency of silica flour reaches 92.1%, and the transformation efficiency of dme reaches 96.5%, and stopped reaction reclaims solvent, finally prepares dimethyl cyclosiloxane product.
Fig. 1 is the process flow sheet that continuous processing is produced dimethyl cyclosiloxane, and Fig. 2 adopts vapor-phase chromatography to detect online the selection rate of DMC with the change curve in reaction times.
After reaction finishes, in conjunction with on-line determination, calculating can obtain the selection rate of reaction product DMC, and silica flour and dimethyl ether conversion rate, as follows:
Above-mentioned example is only explanation technical conceive of the present invention and feature, and its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalent transformations that spirit is done according to the present invention or modification, within all should being encompassed in protection scope of the present invention.
Claims (7)
1. the method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization, is characterized in that, comprises the steps:
(1) dme, monobromethane are derived and entered reactor by pipeline from dme storage tank (2), monobromethane storage tank (3) respectively, wherein, be provided with molecule screen casing to remove the minor amount of water in dme, monobromethane at this pipeline;
(2) in addition by catalyst mixture and the SiO that removes silicon powder surface layer
2silica flour, fully mix postactivatedly according to weight ratio 1～5:100, import to silica flour/catalyst/solvent storage tank (1),
(3) after the activation silica flour of the importing in solvent and step (2) is fully mixed according to weight ratio 1～5:1, add together in reactor (4), airtight, pressure is 0.1～0.3MPa, be warming up to 250 DEG C～320 DEG C, pass into the monobromethane in step (1), the weight ratio of monobromethane and activation silica flour is 0.05～0.15:1, then in reactor, pass into dme continuous measurement, the intake velocity of dme is 10～15 kgs/hr, stirring velocity is 50～100 revs/min, carries out continuous reaction;
(4) mixture that reaction generates is separated and is obtained high boiler material and lower boiling material by separator column, high boiler material passes back into reactor (4), lower boiling material needs further condensation, wherein the methylsiloxane mixture phlegma in lower boiling material enters the first distillation tower (6) successively, the first condenser (7) enters in still kettle (10) and separates and obtain dimethyl cyclosiloxane, in lower boiling material, the complete dme of unreacted and the monobromethane that do not consume are further by second column (11), the second condenser (12) compression is collected, collect respectively incomplete product through different fractions reception storage tank and be again cycled to used in successive reaction.
2. the method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization according to claim 1, is characterized in that, the silica flour of described step (2) is removed the SiO of silicon powder surface layer
2for, take hydrofluoric acid solution and silica flour that weight ratio is 4～6:1, at room temperature stir 0.5～1.5 hour, filter, fully to wash with dehydrated alcohol, vacuum-drying 2～8 hours at 60～90 DEG C, removes the SiO of silicon powder surface layer
2for subsequent use, and silica flour size is 50～250 μ m.
3. the method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization according to claim 1, it is characterized in that, the silica flour activation treatment of described step (2) is cryogenic vacuum pre-treatment or Microwave Pretreatment, cryogenic vacuum pre-treatment is to add in crucible after silica flour and catalyzer are fully ground according to weight ratio 1～5:100, be placed in vacuum drying oven, vacuumize, rising temperature to 80～140 DEG C, are incubated 1～6 hour; Microwave Pretreatment is to add in crucible after silica flour and catalyst mixture are fully ground according to weight ratio 1～5:100, is inserted in microwave oven, and the power of microwave oven is 800-1500W, and the time of microwave treatment is 1～5 minute.
4. the method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization according to claim 1, it is characterized in that, catalyst mixture in the activation treatment of described step (2) is made up of catalyzer and promotor, catalyzer is neutralized verdigris, copper hydroxide, in cuprous chloride a kind of or more than one; Promotor is zinc oxide or tin or its combination, and the weight ratio of catalyzer and promotor is 50:1～3.
5. the method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization according to claim 1, it is characterized in that, solvent in the synthesis step of described dimethyl cyclosiloxane is paraffin oil, dodecylbenzene, two undecyl benzene etc. a kind of or more than one.
6. the method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization according to claim 1, is characterized in that, the weight ratio of the solvent/silica flour in described step (3) is 1～5:1.
7. the method that dimethyl cyclosiloxane is produced in non-halogenated direct serialization according to claim 1, is characterized in that, in described step (3), the synthetic temperature of dimethyl cyclosiloxane is 260 DEG C～300 DEG C.
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| CN109400951A (en) * | 2018-12-29 | 2019-03-01 | 佛山市金银河智能装备股份有限公司 | A kind of production method and device of DMC |
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