CN102838629B - Novel process for synthesizing methyl chlorosilane by methane chloride byproduct chloromethane - Google Patents
Novel process for synthesizing methyl chlorosilane by methane chloride byproduct chloromethane Download PDFInfo
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Abstract
The invention provides a novel process for synthesizing methyl chlorosilane by methane chloride byproduct chloromethane, which belongs to the field of organic silicon production. The process comprises the following steps of: by using activated alumina as a catalyst, carrying out hydrochlorination on methanol and hydrogen chloride in an immobilized reactor; carrying out sulfuric acid washing, dehydration, dealcoholization, compressing and condensing on a reaction product so as to obtain coarse chloromethane; feeding partial coarse chloromethane into a refining system; after the coarse chloromethane is gasified, carrying out water washing, alkali washing, sulfuric acid three-stage drying, compressing and condensing on the gasified coarse chloromethane so as to obtain chloromethane; after the chloromethane is gasified, reacting the chloromethane with silicon powder in a fluidized bed; by using ternary copper as a catalytic system, generating a methyl chlorosilane mixed monomer; refining the methyl chlorosilane mixed monomer so as to separate out dimethyldichlorosilane; carrying out constant boiling acid hydrolysis on the dimethyldichlorosilane so as to obtain polymethylsiloxane and byproduct hydrochloric acid; and cracking the polymethylsiloxane so as to obtain a methylsiloxane mixed cycle body. According to the invention, the methane chloride byproduct chloromethane is used for preparing an organic silicon monomer after being refined and used for achieving industrial cogeneration of methane chloride and organic silicon, so that the production cost is greatly reduced and economic benefits are increased.
Description
Technical field
The invention belongs to a kind of methane chloride byproduct chloromethane of organosilicon production field for methyl chlorosilane new synthetic process.
Background technology
The major product of methane chloride is methylene dichloride and trichloromethane, what adopt is gas-phase methanol method production technique, and methyl alcohol and hydrogenchloride react in fixed-bed reactor produces methyl chloride, with activated alumina as catalyzer, the methyl chloride generated is after sulfuric acid scrubbing, dehydration dealcoholysis, generate thick methyl chloride after compression condensation, purity index is Wt% methyl chloride 96%, methylene dichloride 120ppm, hydrogenchloride 2.5%, thick methyl chloride through gasification after with chlorine reaction, generate methylene dichloride, chloroform and tetracol phenixin.Excessive methyl chloride recycle, this reaction belongs to free radical reaction, a large amount of hydrogenchloride is generated in reaction process, be transported to hydrochlorinate device for the production of methyl chloride, on the basis maintaining line balancing, unnecessary hydrogenchloride be transported to hydrogen chloride absorption device through hydrochlorinate 20% synthesis dilute hydrochloric acid absorb, generate 31% by-product hydrochloric acid.The ratio of methane chloride design methylene dichloride and chloroform can adjust in 40-60% interval, because chloroform is the starting material as organic fluorine, the market requirement is higher than methylene dichloride, such proportion of production most of the time is chloroform: methylene dichloride=6:4, under this ratio condition, the chlorination hydrogen amount in reaction process increases, and unnecessary hydrogenchloride process water absorbs and generates hydrochloric acid, Shandong is the large province of chlor-alkali, and by-product hydrochloric acid selling pressure is very large.After this part hydrogenchloride becomes hydrochloric acid thus, benefit is very low, and operated pressure is large.
First organosilicon production technique is that the hydrochloric acid of 31% is through conventional desorption production hydrogenchloride, hydrogenchloride and gasification of methanol react, the liquor zinci chloridi of 75% makees catalyzer, carry out liquid phase reaction, after refining, generate finished product methyl chloride (Wt%, 99.98%), methyl chloride gasifies afterwards and silica flour reacts in fluidized-bed, using Ternary copper as catalyst system, generate methyl chlorosilane mix monomer, after refining, isolate dimethyldichlorosilane(DMCS), one first, front three, one first is hydrogeneous, high boiling material, the products such as low-boiling-point substance are transported to outside finished product tank field and sell, dimethyldichlorosilane(DMCS) carries out azeotropic acid hydrolysis, hydrolysate is the hydrolyzate (polymethyl siloxane) of methylsiloxane thread and ring, the concentrated hydrochloric acid of by-product 31% simultaneously, concentrated hydrochloric acid is transported to innovation of hydrochloric acid desorption units for the production of hydrogenchloride, complete the inner chlorine circulation of organosilicon, hydrolyzate forms mixed methylcyclosiloxane after carrying out cracking, sell as outside final product.
Methyl chloride purity requirement used in organosilicon production is higher, and therefore market value is also higher, and according to the rule of methyl chloride market value, average price per ton 3500 yuan, therefore production cost is higher.And the by product methyl chloride cost that methane chloride is produced is lower, but its purity does not reach the requirement that organosilicon is produced.
Summary of the invention
The object of the invention is exactly for prior art Problems existing, provides a kind of methane chloride byproduct chloromethane reasonable in design, with low cost for methyl chlorosilane new synthetic process.
The present invention is achieved by the following scheme: with activated alumina as catalyzer, methyl alcohol and hydrogenchloride carry out hydrochlorination in immobilization reactor, after sulfuric acid scrubbing, dehydration dealcoholysis, compression condensation, obtain thick methyl chloride; The thick methyl chloride of a part prepares methylene dichloride and trichloromethane by chlorination reaction, and the byproduct hydrogen chloride part of chlorination reaction is delivered to that immobilization reactor carries out hydrochlorination recycle, another part is delivered to absorption unit and generates by-product hydrochloric acid; Methyl chloride is obtained through washing, alkali cleaning, sulfuric acid three-stage drying, compression condensation after the thick methyl chloride gasification of another part, methyl chloride gasifies afterwards and silica flour reacts in fluidized-bed, using Ternary copper as catalyst system, generate methyl chlorosilane mix monomer, go out dimethyldichlorosilane(DMCS) through refining spearation; It is polymethyl siloxane that dimethyldichlorosilane(DMCS) carries out azeotropic acid hydrolysis, then obtains methylsiloxane mixed methylcyclosiloxane through cracking.
Such scheme can improve further:
Described washing step is: carry out at acid-water washing tower, and wherein thick methyl chloride gas is by air inlet at the bottom of tower, de-salted water by tower top charging, and the dilute hydrochloric acid that at the bottom of tower, absorption obtains is squeezed into tower top by recycle pump and recycled; Described caustic wash process is: carry out at soda-wash tower, and alkali lye adopts 20% sodium hydroxide solution, and in soda-wash tower tower reactor, liquid level is by governor valve control, and in tower, alkali lye is cooled to 5 ~ 10 DEG C by alkali water cooler and recycles; Described sulfuric acid three-stage drying operation is: after soda-wash tower mist eliminator, enter three-stage drying tower by soda-wash tower tower top thick methyl chloride out successively, recycle sulfuric acid is reverse enters three-stage drying tower, discharged by the dry tower top of the third stage after thick methyl chloride drying, then after mist eliminator, enter the surge tank of suction port of compressor, recycle sulfuric acid enters Waste Sulfuric Acid storage tank by discharging at the bottom of the tower of the first drying tower through sulfuric acid transferpump; Described compression condensation operation is: by the methyl chloride gas come by suction port of compressor surge tank, enter methyl chloride compressor compresses to 0.5 ~ 0.8MPa, then methyl chloride condenser is entered, to congeal into liquid with recirculated water cooling in methyl chloride condenser, methyl chloride enters methyl chloride tundish, uncooled gas phase of getting off enters methyl chloride tail gas condenser, enters methyl chloride tundish for subsequent use after the condensation of spent glycol solution gets off to become liquid.
Stored by thick methyl chloride storage tank after compression condensation, and be transported to the thick methyl chloride storage tank of refining system by tank car; Wherein during entrucking, tank car gas phase and thick methyl chloride storage tank gas phase access thick methyl chloride exhaust condenser system, pass through-35 DEG C of freonll-11 condensations; Adopt scraping blade pump when unloading, scraping blade adopts fluoroplastics material, and when unloading, tank car gas phase and thick methyl chloride storage tank gas phase connect into thick methyl chloride condenser system, passes through the refrigerant cooling of-15 DEG C.
Described by-product hydrochloric acid produces hydrogenchloride through desorption, and hydrogenchloride and gasification of methanol make catalyzer carry out liquid phase reaction with the liquor zinci chloridi of 75%, after refining, generate methyl chloride; Methyl chloride gasifies afterwards and silica flour reacts in fluidized-bed, using Ternary copper as catalyst system, generates methyl chlorosilane mix monomer, goes out dimethyldichlorosilane(DMCS) through refining spearation; It is polymethyl siloxane that dimethyldichlorosilane(DMCS) carries out azeotropic acid hydrolysis, then obtains methylsiloxane mixed methylcyclosiloxane through cracking.
For the preparation of organosilane monomer after the present invention is refining thick for methane chloride by-product methyl chloride, and realize methane chloride and silicone industry coproduction, greatly reduce production cost, improve economic benefit.
Embodiment
Below in conjunction with the practical situation of our company, the present invention is described further.The existing methane chloride of our company 360,000 tons (single 40,000 tons, cover, 9 covers), organosilane monomer 120,000 tons (single cover), production technique is as follows:
The major product of methane chloride is methylene dichloride and trichloromethane, what adopt is gas-phase methanol method production technique, and methyl alcohol and hydrogenchloride react in fixed-bed reactor produces methyl chloride, with activated alumina as catalyzer, the methyl chloride generated is after sulfuric acid scrubbing, dehydration dealcoholysis, generate thick methyl chloride after compression condensation, purity index is Wt% methyl chloride 96%, methylene dichloride 120ppm, hydrogenchloride 2.5%, thick methyl chloride through gasification after with chlorine reaction, generate methylene dichloride, chloroform and tetracol phenixin.Excessive methyl chloride recycle, this reaction belongs to free radical reaction, a large amount of hydrogenchloride is generated in reaction process, be transported to hydrochlorinate device for the production of methyl chloride, on the basis maintaining line balancing, unnecessary hydrogenchloride be transported to hydrogen chloride absorption device through hydrochlorinate 20% synthesis dilute hydrochloric acid absorb, generate 31% by-product hydrochloric acid.
The ratio of methane chloride design methylene dichloride and chloroform can adjust in 40-60% interval, because chloroform is the starting material as organic fluorine, the market requirement is higher than methylene dichloride, such proportion of production most of the time is chloroform: methylene dichloride=6:4, under this ratio condition, the chlorination hydrogen amount in reaction process increases, and unnecessary hydrogenchloride process water absorbs and generates hydrochloric acid, Shandong is the large province of chlor-alkali, and by-product hydrochloric acid selling pressure is very large.After this part hydrogenchloride becomes hydrochloric acid thus, benefit is very low, and operated pressure is large.
Organic Silicon Plant scale is 120,000/year, first production technique is that the hydrochloric acid of 31% is through conventional desorption production hydrogenchloride, hydrogenchloride and gasification of methanol react, the liquor zinci chloridi of 75% makees catalyzer, carry out liquid phase reaction, after refining, generate finished product methyl chloride (Wt%, 99.98%), methyl chloride gasifies afterwards and silica flour reacts in fluidized-bed, using Ternary copper as catalyst system, generate methyl chlorosilane mix monomer, after refining, isolate dimethyldichlorosilane(DMCS), one first, front three, one first is hydrogeneous, high boiling material, the products such as low-boiling-point substance are transported to outside finished product tank field and sell, dimethyldichlorosilane(DMCS) carries out azeotropic acid hydrolysis, hydrolysate is the hydrolyzate of methylsiloxane thread and ring, the concentrated hydrochloric acid of by-product 31% simultaneously, concentrated hydrochloric acid is transported to innovation of hydrochloric acid desorption units for the production of hydrogenchloride, complete the inner chlorine circulation of organosilicon, hydrolyzate forms mixed methylcyclosiloxane after carrying out cracking, sell as outside final product.
Methyl chloride EQUILIBRIUM CALCULATION FOR PROCESS is carried out to methane chloride device and Organic Silicon Plant below
One, Organic Silicon Plant methyl chloride demand EQUILIBRIUM CALCULATION FOR PROCESS
Organosilane monomer device is by annual output 120000 tons of crude monomers, within 7200 hours, calculate, the amount of product crude monomer per hour is 16.7 tons (wherein dimethyldichlorosilane(DMCS) average content is 84%), empirical value methyl chloride/crude monomer=0.85, need the amount of total methyl chloride be 16.7*0.85=14.2 ton/hour.
Wherein dimethyldichlorosilane(DMCS) hydrolysis produces hydrogenchloride, returns organosilicon production technique and produces methyl chloride, according to hydrolysis hydrogenchloride yield 99%, when not dark desorption, and hydrogenchloride/methyl chloride=0.84, namely
Hydrolysis produces the amount of hydrogenchloride: 16.7*0.84*71/129*36.5/35.5*99%=7.86t/h, generates the amount 7.86/0.84=9.3 ton of methyl chloride, so need every day the amount of supplementary methyl chloride for (14.2-9.3) * 24=118 ton.
Two, methane chloride device EQUILIBRIUM CALCULATION FOR PROCESS
According to actual operating data, ensure that synthesis dilute hydrochloric acid fully absorbs into the concentrated acid of 31%, under the condition that hydrochlorinate device processing power is enough, the every covering device of methane chloride thick methyl chloride 15 tons more than needed per hour.Existing 9 covering devices, 15*9*0.96=130 ton, namely needs the 118 tons of methyl chloride supplemented to adopt the byproduct chloromethane of methane chloride production line to refine to provide every day.
To achieve these goals, in the situation that the technical process keeping methane chloride and organosilicon to produce is constant, following technical scheme is increased:
1, amplify methane chloride hydrochlorination device, increase packed catalyst amount, improve thick methyl chloride production capacity;
Hydrochlorination device is transformed, brings up to 2.4 meters by former Process Design Package diameter 2.1m, improve the treatment capacity of reaction methyl chloride synthesis;
2, the newly-increased thick methyl chloride loading apparatus of design;
Loading platform is increased at methane chloride device, because containing the hydrogenchloride of 2.5% in thick methyl chloride, not easily condensation, in design process, tank car gas phase and thick methyl chloride gas phase access thick methyl chloride exhaust condenser system, with-35 DEG C of freonll-11 condensations, ensure the pressure equilibrium of entrucking.
3, at the newly-increased unloading unit of Organic Silicon Plant design
First on unloading unit, select scraping blade pump, the pump not easily cavitation of this kind of model, scraping blade adopts strengthens fluoroplastics material, safe and reliable, gas phase and methyl chloride storage tank gas phase are connected, access methyl chloride condenser system, adopt the low temperature refrigerant of-15 DEG C to cool, ensure that methyl chloride is unloaded smoothly.
4, thick methyl chloride refining plant is designed at Organic Silicon Plant.
Newly-increased methyl chloride gasification, washing, alkali cleaning, sulfuric acid three-stage drying, compression condensation device.
After thick methyl chloride gasification, enter acid-water washing system, de-salted water enters in tower by acid-water washing column overhead, carries out mass transfer, in order to absorb the hydrogenchloride in methyl chloride with thick methyl chloride reverse contact in tower.Dilute hydrochloric acid out at the bottom of tower enters tower internal recycle through recycle pump by acid-water washing column overhead and uses.
Acid-water washing column overhead thick methyl chloride gas out goes soda-wash tower tower reactor, removes the hydrogenchloride in methyl chloride by acid-base neutralisation principle further.With the thick methyl chloride reverse hydrogenchloride contacting to neutralize in gas in tower come from tower reactor.Tower reactor liquid level governor valve control, delivers to soda-wash tower tower reactor water cooler by soda-wash tower recycle pump and is cooled to 5 ~ 10 DEG C, recycle; Waste lye enters treatment unit for waste water through pump.
The top delivering to soda-wash tower from the alkali lye batch tank concentration sodium hydroxide alkali lye fresh feed pump that is 20% enters in tower.
By soda-wash tower top thick methyl chloride out (containing methyl chloride, methyl alcohol, dme, water etc.) after soda-wash tower mist eliminator, enter first step drying tower again and carry out reverse contact with the sulfuric acid recycled under tower, mainly except to anhydrate and after the impurity such as methyl alcohol, dme, drying tower bottom, the second stage is entered from its top, carry out reverse contact with the sulfuric acid recycled under tower again to absorb further, entering third stage drying tower again carries out after reverse contact with fresh sulfuric acid, forms the refining methyl chloride that purity reaches 99.99%.Gas by third stage drying tower top out, enters third stage drying tower mist eliminator, enters suction port of compressor surge tank after removing the fluid sulphuric acid that may carry secretly.
98%(winter 95% of being come by sulfuric acid tank field) sulfuric acid directly enter third stage drying tower through sulfuric acid pump.
Recycle sulfuric acid recycles by by overflowing to successively in the second stage, the first step under tower, conducts heat at tower inner transmission matter with the methyl chloride gas entered from tower bottom, the impurity in removing methyl chloride gas.
Bottom first step drying tower, 80%(winter is out 75%) sulfuric acid sell outside Waste Sulfuric Acid tank field through pump delivery.
The methyl chloride gas come by suction port of compressor surge tank, enter methyl chloride compressor compresses to 0.5 ~ 0.8MPa, then methyl chloride condenser is entered, to congeal into liquid with recirculated water cooling in methyl chloride condenser, methyl chloride enters methyl chloride tundish, uncooled gas phase of getting off enters methyl chloride tail gas condenser, enters methyl chloride tundish after the condensation of spent glycol solution gets off to become liquid, after pump metering, deliver to methyl chlorosilane synthesis unit.
Three, technical economical analysis
Cost refined by thick methyl chloride
| Sequence number | Title | Unit price (unit) | Unit consumption | Cost (unit) |
| 1 | Methyl alcohol | 2800 | 0.65 | 1820 |
| 1 | Electricity | 0.78 | 150 degree | 117 |
| 2 | Steam | 200 | 1.3 ton | 260 |
| 3 | Liquid caustic soda | 600 | 0.0236 | 15 |
| 4 | Sulfuric acid | 565 | 0.0397 | 22 |
| 5 | Freight charges | 60 | 1 | 60 |
| Add up to | 2294 |
Cost 2294 yuan/ton refined by thick methyl chloride, and through adjusting, by methane chloride by-product hydrochloric acid 80 yuan/ton calculating, the cost that methane chloride by-product hydrochloric acid is converted to methyl chloride is 480 yuan.
That is: the cost of methyl chloride is 2774 yuan.
According to the rule of methyl chloride market value, average price per ton 3500 yuan.I.e. saving per ton 726 yuan compared with methyl chloride outsourcing.The outsourcing amount of annual methyl chloride is 3.54 ten thousand tons, 35400*0.0726=2570 ten thousand yuan.
Existing apparatus cost-saving 2,570 ten thousand yuan every year, benefit is obvious, and synthesizes actual motion by methyl chlorosilane, and methyl chlorosilane monomer quality does not change, operational excellence.And methyl chloride supply is stablized, produce and do not affect by outside methyl chloride market fluctuation.
Claims (1)
1. a methane chloride byproduct chloromethane is used for methyl chlorosilane new synthetic process, it is characterized in that: with activated alumina as catalyzer, methyl alcohol and hydrogenchloride carry out hydrochlorination in immobilization reactor, after sulfuric acid scrubbing, dehydration dealcoholysis, compression condensation, obtain thick methyl chloride; The thick methyl chloride of a part prepares methylene dichloride and trichloromethane by chlorination reaction, and the byproduct hydrogen chloride part of chlorination reaction is delivered to that immobilization reactor carries out hydrochlorination recycle, another part is delivered to absorption unit and generates by-product hydrochloric acid; Refining system delivered to by the thick methyl chloride of another part, methyl chloride is obtained through washing, alkali cleaning, sulfuric acid three-stage drying, compression condensation after thick methyl chloride gasification, methyl chloride gasifies afterwards and silica flour reacts in fluidized-bed, using Ternary copper as catalyst system, generate methyl chlorosilane mix monomer, go out dimethyldichlorosilane(DMCS) through refining spearation; It is polymethyl siloxane and by-product hydrochloric acid that dimethyldichlorosilane(DMCS) carries out azeotropic acid hydrolysis, and then polymethyl siloxane obtains methylsiloxane mixed methylcyclosiloxane through cracking; Described washing step is: carry out at acid-water washing tower, and wherein thick methyl chloride gas is by air inlet at the bottom of tower, de-salted water by tower top charging, and the dilute hydrochloric acid that at the bottom of tower, absorption obtains is squeezed into tower top by recycle pump and recycled; Described caustic wash process is: carry out at soda-wash tower, and alkali lye adopts 20% sodium hydroxide solution, and in soda-wash tower tower reactor, liquid level is by governor valve control, and in tower, alkali lye is cooled to 5 ~ 10 DEG C by alkali water cooler and recycles; Described sulfuric acid three-stage drying operation is: after soda-wash tower mist eliminator, enter three-stage drying tower by soda-wash tower tower top thick methyl chloride out successively, recycle sulfuric acid is reverse enters three-stage drying tower, discharged by the dry tower top of the third stage after thick methyl chloride drying, then after mist eliminator, enter the surge tank of suction port of compressor, recycle sulfuric acid enters Waste Sulfuric Acid storage tank by discharging at the bottom of the tower of the first drying tower through sulfuric acid transferpump; Described compression condensation operation is: by the methyl chloride gas come by suction port of compressor surge tank, enter methyl chloride compressor compresses to 0.5 ~ 0.8MPa, then methyl chloride condenser is entered, to congeal into liquid with recirculated water cooling in methyl chloride condenser, methyl chloride enters methyl chloride tundish, uncooled gas phase of getting off enters methyl chloride tail gas condenser, enters methyl chloride tundish for subsequent use after the condensation of spent glycol solution gets off to become liquid; Stored by thick methyl chloride storage tank after compression condensation, and be transported to the thick methyl chloride storage tank of refining system by tank car; Wherein during entrucking, tank car gas phase and thick methyl chloride storage tank gas phase access thick methyl chloride exhaust condenser system, pass through-35 DEG C of freonll-11 condensations; Adopt scraping blade pump when unloading, scraping blade adopts fluoroplastics material, and when unloading, tank car gas phase and thick methyl chloride storage tank gas phase connect into thick methyl chloride condenser system, passes through the refrigerant cooling of-15 DEG C; The by-product hydrochloric acid of described azeotropic acid hydrolysis produces hydrogenchloride through desorption after desorb, and hydrogenchloride and gasification of methanol make catalyzer carry out liquid phase reaction with the liquor zinci chloridi of 75%, after refining, generate methyl chloride; Methyl chloride gasifies afterwards and silica flour reacts in fluidized-bed, using Ternary copper as catalyst system, generates methyl chlorosilane mix monomer, goes out dimethyldichlorosilane(DMCS) through refining spearation; It is polymethyl siloxane that dimethyldichlorosilane(DMCS) carries out azeotropic acid hydrolysis, then obtains methylsiloxane mixed methylcyclosiloxane through cracking; The by-product hydrochloric acid of described chlorination reaction produces hydrogenchloride through desorption, and hydrogenchloride and gasification of methanol make catalyzer carry out liquid phase reaction with the liquor zinci chloridi of 75%, after refining, generate methyl chloride; Methyl chloride gasifies afterwards and silica flour reacts in fluidized-bed, using Ternary copper as catalyst system, generates methyl chlorosilane mix monomer, goes out dimethyldichlorosilane(DMCS) through refining spearation; It is polymethyl siloxane that dimethyldichlorosilane(DMCS) carries out azeotropic acid hydrolysis, then obtains methylsiloxane mixed methylcyclosiloxane through cracking.
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| CN106008151A (en) * | 2016-07-22 | 2016-10-12 | 合盛硅业股份有限公司 | Methyl chloride synthesis method |
| CN112898115B (en) * | 2018-06-28 | 2022-05-31 | 湖北兴瑞硅材料有限公司 | Process for synthesizing chloromethane from hydrogen chloride under pressure |
| CN110590828A (en) * | 2019-09-26 | 2019-12-20 | 合盛硅业股份有限公司 | Methyl chlorosilane synthesis equipment and parking method |
| CN111675196B (en) * | 2020-07-08 | 2022-03-11 | 镇江江南化工有限公司 | Method for treating hydrogen chloride generated by hydrolysis of chlorosilane through enhanced condensation by using chloromethane as refrigerant |
| CN111747822A (en) * | 2020-07-28 | 2020-10-09 | 安徽东至广信农化有限公司 | Process for recovering methyl chloride from glyphosate tail gas |
| CN112645976A (en) * | 2020-12-23 | 2021-04-13 | 浙江天采云集科技股份有限公司 | Method for preparing methyl chlorosilane organic silicon by using tail gas FTrPSA (fluorine-doped polysilicon-fluoride) in growth process of chlorine-based CVD (chemical vapor deposition) crystal film |
| CN113828001B (en) * | 2021-10-29 | 2022-10-11 | 新疆晶硕新材料有限公司 | Separation system and separation method of chloromethane |
| CN114130345A (en) * | 2021-12-14 | 2022-03-04 | 福建立亚化学有限公司 | Preparation method of polydimethylsilane |
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