CN103183827B - A kind of organochlorosilane continuous print Concentrated acid hydrolysis method - Google Patents
A kind of organochlorosilane continuous print Concentrated acid hydrolysis method Download PDFInfo
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Abstract
The present invention relates to a kind of organochlorosilane continuous print Concentrated acid hydrolysis method, comprise step: (1) organochlorosilane and concentrated acid are hydrolyzed to react and generate the higher hydrochloric acid of concentration and thick hydrolyzate in hydrolysis reactor; (2) liquid generated after hydrolysis reaction is after coarse separator, and concentrated acid enters falling-film evaporator, and heat exchange generates HCl gas, obtains the HCl gas produced for methyl chloride; Concentrated acid at the bottom of tower enters hydrolysis reactor and recycles; The oil phase be separated through coarse separator enters one-level and divides mutually and divide mutually with secondary, isolated acid solution backwater solution reactor cycles, and oil phase then enters follow-up washing step; (3) first the oil phase entering washing step is washed through two-stage series connection and is separated, then enters sig water circulation cleaning and be separated, and finally enters two-stage series connection washing and is separated; Oil phase after washing is oligomeric siloxane products.
Description
Technical field
The present invention relates to technical field of organic silicon production, especially relate to the continuous Concentrated acid hydrolysis of organochlorosilane, generate the processing method of oligosiloxane and anhydrous hydrogen chloride.
Background technology
Organochlorosilane changes intermediate oligoorganosiloxanes that is linear or ring texture into by hydrolysis and polycondensation, is the basis of synthesis silicone oil, silicon rubber, silicone resin.Especially dimethyldichlorosilane(DMCS) (hereinafter referred to as diformazan) is considered to most suitable and is hydrolyzed and condensation reaction with this.
Current domestic diformazan hydrolysis adopts azeotropic acid hydrolysis process mostly.Because resultant hydrogenchloride is dissolved in diluted acid, release a large amount of heat, for making temperature of reaction remain within processing condition requirement, heat need be shifted out, this part heat can not be used in follow-up operation, thus consumes a large amount of energy.In addition, for the hydrogenchloride in recovered acid make its meet methyl chloride synthesis requirement, and be convenient to conveying also to consume a lot of energy.In the postprocessing working procedures of product oligosiloxane, also to produce a large amount of waste water and spent acid, to environment.
French Patent FR2518099 water saturation hydrochloric acid hydrolysis organochlorosilane in shortage, makes the hydrogen chloride gas produced easily process.But hydrolysis not exclusively when water is not enough, the linear polyorganosiloxane comprising Cl in end position namely can be produced.The high chlorine contents of thick hydrolyzate makes the aftertreatment difficulty of product.
It is minimum for 35%(wt that US Patent No. 4382145 applies concentration) water in hydrochloric acid is as reaction water, and its consumption is 10 ~ 30 times (mol ratios) of organochlorosilane, uses at the inner-outer circulation of reactor; US Patent No. 4497942 by concentration be under pressure water in the hydrochloric acid of 40 ~ 42% as reaction water, consumption is 10 ~ 50 times (mol ratios) of organochlorosilane, and hydrochloric acid uses at reactor inner-outer circulation.The advantage of two patents directly obtains anhydrous hydrogen chloride, saved energy, but there is the incomplete shortcoming of hydrolysis, and do not provide the data of hydrolyzate and hydrogenchloride yield and purity.
US Patent No. 6225490 discloses the hydrolysis process of continuous print organochlorosilane, and this hydrolysis process comprises at least three sections of reaction series connection, and each section of reaction all comprises independently reactor and phase separator.Organochlorosilane adds from first paragraph reactor, and reaction water is all provided by the feed water of final stage, and first paragraph reaction produces hydrogen chloride gas.The hydrolyzate that leading portion produces enters next section and to be hydrolyzed process, and the hydrochloric acid that back segment produces is delivered to leading portion again and reacted, and namely have employed three sections of reflux types and to be hydrolyzed reaction.Although this technique can produce hydrogen chloride gas, the hypotony of gas phase chlorination hydrogen, should not directly apply in synthesis methyl chloride.And due to this technique serial operation, therefore turndown ratio is little, the reaction of any a section is not up to standard, all will affect the final quality of product.
US Patent No. 6326452 discloses the method for hydrolysis of organochlorosilane, mainly comprises two steps: the first step is actual is that the water of applied chemistry metering makes hydrolyzing organochlorosilanes generating portion with the thick hydrolysate of the organopolysiloxane of Cl end-blocking and hydrogen chloride gas; Quantitative high-temperature steam is carried out air lift to thick hydrolyzate by second step, reduce chlorinity and generate hydrochloric acid turn back to the first step reaction keep the skin wet, unnecessary hydrochloric acid then removes the hydrogen chloride gas parsing low pressure, and this gas should not be applied in the synthesis of methyl chloride.And thick product adopts steam-treated, the viscosity of hydrolyzate is final also restive.
Comprehensive above-mentioned patent and document known, continuous hydrolyzing organochlorosilanes technique reasonable in design is necessary, this technique should obtain has enough pressure with dry HCl gas to be directly used in the synthesis of methyl chloride, and this technique should reduce the generation of waste liquid as far as possible, viscosity and the cl content of final organo-siloxane reach requirement, can stably operate and control.
Summary of the invention
Technical purpose of the present invention, is to overcome the shortcoming and defect in above-mentioned processing method, provides that a kind of stable operation, energy consumption are little, continuous print organochlorosilane Concentrated acid hydrolysis processing method.Hydrolyzate yield is 95-98%(wt%), the yield of dry HCl gas is 94-98%(wt%).
In order to achieve the above object, the technical solution used in the present invention is:
A kind of organochlorosilane continuous print Concentrated acid hydrolysis method, comprises step:
(1) organochlorosilane and concentrated acid are hydrolyzed to react and generate the higher hydrochloric acid of concentration and thick hydrolyzate in hydrolysis reactor, in reaction system, the mol ratio of water and organochlorosilane is 5:1 ~ 20:1, temperature of reaction 20 ~ 50 DEG C, working pressure is gauge pressure 0.1 ~ 0.5MPa, and organochlorosilane and the concentrated acid residence time in hydrolysis reactor is 60 ~ 180s;
(2) liquid generated after hydrolysis reaction is after coarse separator, concentrated acid enters falling-film evaporator, heat exchange generates HCl gas, enter dry and impurity removing equipment through the tower top of vaporizer again and remove impurity in HCl gas and moisture, pressure is 0.2 ~ 0.5MPa, obtains the HCl gas produced for methyl chloride; Concentrated acid at the bottom of tower enters hydrolysis reactor and recycles; The oil phase be separated through coarse separator enters one-level and divides mutually and divide mutually with secondary, isolated acid solution backwater solution reactor cycles, and oil phase then enters follow-up washing step;
(3) first the oil phase entering washing step is washed through two-stage series connection and is separated, and wash soft water used and quantitatively add, washing temperature is 50 ~ 90 DEG C, and the volume ratio of water and oil phase is 0.5:1 ~ 3:1, and working pressure is 0.1 ~ 0.3MPa; The diluted acid that washing produces enters hydrolysis reactor supplementing as water source;
(4) oil phase after two-stage washing enters sig water circulation cleaning and being separated, and sig water is the sodium carbonate solution of 4 ~ 20%wt, and the volume ratio of alkali lye and oil phase is 2:1 ~ 8:1, to remove acid in oil phase and most free chlorines; Alkali lye after separation recycles;
(5) in step (4), isolated oil phase enters last two-stage series connection washing and is separated, and soft water quantitatively adds, and the aqueous phase major part after separation is for preparing sig water, and small part enters salkali waste flow container; Oil phase after washing is oligomeric siloxane products.
Method for hydrolysis of the present invention, the wherein anhydrous cleaning of gained hydrogen chloride gas in step (2), pressure is 0.2 ~ 0.5MPa.
Method for hydrolysis of the present invention, the drying wherein in step (2) and impurity removing equipment are the conventional equipment can removing impurity in HCl gas and moisture, as HCl lyophilization system and circulation whirlwind scum dredger (also known as circulation type mist eliminator) etc.
Method for hydrolysis of the present invention, wherein in step (3), the water consumption of washing water used is at most that this part water is participated in the reaction be hydrolyzed completely.
Method for hydrolysis of the present invention, wherein in step (1), hydrolysis reactor is the reflection equipment that organochlorosilane and concentrated acid can be made wherein to react, be preferably the dispersion liquid membrane type Analytic Tower that efficiency is higher, described dispersion liquid membrane type Analytic Tower comprises shell, and described shell is with bearing, upper cover hypocentrum, flange, outer cylinder body and is connected as a single entity by fastening piece and seals; Also inner barrel is comprised in described shell; The top of described Analytic Tower has fluid inlet, and bottom has liquid outlet, and the side direction at outer cylinder body is opened in air outlet; Liquid distributing board is installed with between upper cover and outer cylinder body, it is splashproof silk screen above liquid distributing board, it is the film-forming plates of proper alignment below liquid distributing board, film-forming plates is horizontal support, totally 3 ~ 10 layers, the angle becoming template and horizontal plane is 15 ~ 75 degree, and between layers, film-forming plates misorientation arranges; All film-forming plates are all arranged among inner barrel, form the guide passage of annular space as gas between inner barrel and outer cylinder body.The residence time 60 ~ 120s.
The preferred dimethyldichlorosilane(DMCS) of raw material organochlorosilane of the present invention, but do not refer in particular to as dimethyldichlorosilane(DMCS).
Method of the present invention, one of major technique effect makes to be hydrolyzed the HCl gas produced by suitable reaction pressure (0.1 ~ 0.5MPa gauge pressure) enough pressure, utilize the impurity in three grades of integrated HCl lyophilization systems and scum dredger device removing HCl gas and moisture simultaneously, make HCl gas drying and pure, to meet the synthesis requirement of methyl chloride.
Another technique effect of present method utilizes the superstoichiometric water (water in concentrated acid: organochlorosilane=5 ~ 20:1, mol ratio) and suitable temperature of reaction (20 ~ 50 DEG C) Water Under solution, and by improving the structure of reactor, water-oil phase film forming contacts, the product after being hydrolyzed is made to there are not Si-Cl remnants as far as possible, to reduce the water consumption in subsequent handling, avoid producing diluted acid waste liquid.
3rd technique effect of present method utilizes the strict water and the sig water (water: organopolysiloxane=2 ~ 8:1 that control metering, volume ratio) Pyatyi carrying out washing treatment is carried out to product, organopolysiloxane is made to have low viscosity (≤16cP) and low free Cl content (≤6ppm), and stable and controllable for quality.Waste lye quantity discharged is down to minimum, for the make up water of hydrolysis reaction in a small amount of diluted acid Returning reactor that washing produces.
Following excellent hydrolysis effect can be shown by the enforcement of above-mentioned process program of the present invention:
1, the special construction (dispersion liquid membrane type Analytic Tower) of hydrolysis device adds the residence time of hydrolysis, is that water molecules fully contacts with the molecule of organochlorosilane, makes hydrolysis reaction complete.
2, adopt superstoichiometric water to decrease and generate the chloride linear siloxane of end, improve hydrolyzate yield and after reducing
The water consumption of process.And ensure that the temperature variation in reaction process is very little, improve the quality of product organo-siloxane.
The diluted acid produced in washing step recycles the generation avoiding a large amount of spent acid solution, and ensure that the water consumption of the hydrolysis of chlorosilane.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention; Wherein: 1: hydrolysis reactor; 2: coarse separator; 3: falling-film evaporator; 4: phase separator; 5: condenser; 6: circulation type mist eliminator; 7: washing mixing and separating device; 8: alkali cleaning mixing and separating device; 9: washing mixing and separating device; 10: salkali waste tank; 11: chlorosilane entrance; 12:HCl exports; 13: steam inlet; 14: oligosiloxane exports.
Embodiment
For further illustrating the present invention, illustrate with the following Examples:
Below in conjunction with the technical process of Fig. 1 and embodiment, the present invention will be further described, but be not limited thereto.The concentration of hydrochloric acid wherein entering hydrolysis reactor is 33%-38%wt, and the concentration of hydrochloric acid of hydrolysis reactor outlet is 40%-50%wt.
Embodiment 1: dimethyldichlorosilane(DMCS) and concentrated acid enter hydrolysis reactor 1 and be hydrolyzed and react, in reaction system, the mol ratio of water and dimethyldichlorosilane(DMCS) is 5:1, water source is from hydrolyzate oligosiloxane washing step, and concentrated acid recycles between hydrolysis reactor 1 and falling-film evaporator 3.Controlling temperature of reaction is 30 DEG C, working pressure 0.4MPa, residence time 60s.Front two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 0.5:1, and service temperature 55 DEG C, working pressure is 0.1MPa.Alkali cleaning adopts the volume ratio of sig water and oligosiloxane to be 8:1, and service temperature 55 DEG C, working pressure is 0.1MPa.Rear two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 1:1, service temperature 70 DEG C, working pressure 0.1MPa.The index of products therefrom is as follows: the acid content 1.5-2.6%wt in acidic hydrolysis thing, and viscosity is 6-9cP; Through front secondary washing series-connection, alkali cleaning, after two-stage series connection washing after, hydrolyzate be neutrality, viscosity 15 ± 3cP(25 DEG C), hydrolyzate yield is 97.5%wt, cyclics content is 40 ± 5%wt, and hydrogenchloride productive rate is 97%wt, and this hydrolyzate quality meets the requirement of subsequent technique.
Embodiment 2: dimethyldichlorosilane(DMCS) and concentrated acid enter hydrolysis reactor and be hydrolyzed and react, in reaction system, the mol ratio of water and dimethyldichlorosilane(DMCS) is 10:1, water source is from hydrolyzate oligosiloxane washing step, and concentrated acid recycles between hydrolysis reactor and falling-film evaporator.Controlling temperature of reaction is 20 DEG C, working pressure 0.3MPa, residence time 90s.Front two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 2:1, and service temperature 75 DEG C, working pressure is 0.2MPa.Alkali cleaning adopts the volume ratio of sig water and oligosiloxane to be 6:1, and service temperature 65 DEG C, working pressure is 0.1MPa.Rear two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 1:1, service temperature 60 DEG C, working pressure 0.3MPa.The index of products therefrom does not have considerable change.
Embodiment 3: dimethyldichlorosilane(DMCS) and concentrated acid enter hydrolysis reactor and be hydrolyzed and react, in reaction system, the mol ratio of water and dimethyldichlorosilane(DMCS) is 15:1, water source is from hydrolyzate oligosiloxane washing step, and concentrated acid recycles between hydrolysis reactor and falling-film evaporator.Controlling temperature of reaction is 40 DEG C, working pressure 0.2MPa, residence time 1200s.Front two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 3:1, and service temperature 60 DEG C, working pressure is 0.1MPa.Alkali cleaning adopts the volume ratio of sig water and oligosiloxane to be 4:1, and service temperature 60 DEG C, working pressure is 0.2MPa.Rear two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 3:1, service temperature 70 DEG C, working pressure 0.2MPa.The index of products therefrom does not have considerable change.
Embodiment 4: dimethyldichlorosilane(DMCS) and concentrated acid enter hydrolysis reactor and be hydrolyzed and react, in reaction system, the mol ratio of water and dimethyldichlorosilane(DMCS) is 20:1, water source is from hydrolyzate oligosiloxane washing step, and concentrated acid recycles between hydrolysis reactor and falling-film evaporator.Controlling temperature of reaction is 50 DEG C, working pressure 0.3MPa, residence time 60s.Front two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 0.5:1, and service temperature 60 DEG C, working pressure is 0.1MPa.Alkali cleaning adopts the volume ratio of sig water and oligosiloxane to be 8:1, and service temperature 60 DEG C, working pressure is 0.1MPa.Rear two-stage series connection washing adopts the volume ratio of water and oligosiloxane to be 2:1, service temperature 60 DEG C, working pressure 0.1MPa.The index of products therefrom does not have considerable change.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that the common engineering technical personnel in this area make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determine.
Claims (1)
1. an organochlorosilane continuous print Concentrated acid hydrolysis method, comprises step:
(1) organochlorosilane and concentrated acid are hydrolyzed to react and generate the higher hydrochloric acid of concentration and thick hydrolyzate in hydrolysis reactor, in reaction system, the mol ratio of water and organochlorosilane is 5:1 ~ 20:1, temperature of reaction 20 ~ 50 DEG C, working pressure is gauge pressure 0.1 ~ 0.5MPa, and organochlorosilane and the concentrated acid residence time in hydrolysis reactor is 60 ~ 180s; Hydrolysis reactor is dispersion liquid membrane type Analytic Tower, the residence time 60 ~ 120s;
(2) liquid generated after hydrolysis reaction is after coarse separator, concentrated acid enters falling-film evaporator, heat exchange generates HCl gas, enter dry and impurity removing equipment through the tower top of vaporizer again and remove impurity in HCl gas and moisture, pressure is 0.2 ~ 0.5MPa, obtain the HCl gas produced for methyl chloride, the anhydrous cleaning of gained hydrogen chloride gas, pressure is 0.2 ~ 0.5MPa; Concentrated acid at the bottom of tower enters hydrolysis reactor and recycles; The oil phase be separated through coarse separator enters one-level and divides mutually and divide mutually with secondary, isolated acid solution backwater solution reactor cycles, and oil phase then enters follow-up washing step;
(3) first the oil phase entering washing step is washed through two-stage series connection and is separated, and wash soft water used and quantitatively add, washing temperature is 50 ~ 90 DEG C, and the volume ratio of water and oil phase is 0.5:1 ~ 3:1, and working pressure is 0.1 ~ 0.3MPa; The diluted acid that washing produces enters hydrolysis reactor supplementing as water source; The water consumption of washing water used is at most make this part water participate in the reaction be hydrolyzed completely;
(4) oil phase after two-stage washing enters sig water circulation cleaning and being separated, and sig water is the sodium carbonate solution of 4 ~ 20%wt, and the volume ratio of alkali lye and oil phase is 2:1 ~ 8:1, to remove acid in oil phase and most free chlorines; Alkali lye after separation recycles;
(5) in step (4), isolated oil phase enters last two-stage series connection washing and is separated, and soft water quantitatively adds, and the aqueous phase major part after separation is for preparing sig water, and small part enters salkali waste flow container; Oil phase after washing is oligomeric siloxane products.
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| CN103408761B (en) * | 2013-08-09 | 2016-01-20 | 合盛硅业股份有限公司 | A kind of Concentrated acid hydrolysis dimethyldichlorosilane(DMCS) prepares the method for polydimethylsiloxane |
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| CN106006557B (en) * | 2016-05-18 | 2018-06-15 | 昆明理工大学 | A kind of method of chlorosilane raffinate production hydrogen chloride gas |
| CN106279248B (en) * | 2016-08-16 | 2018-09-28 | 湖北兴发化工集团股份有限公司 | A method of preparing neutral organosilicon hydrolyzation object |
| CN108484658B (en) * | 2018-05-28 | 2020-09-25 | 宜昌兴越新材料有限公司 | Production method of hexamethyldisiloxane |
| CN110183479B (en) * | 2019-06-17 | 2020-08-04 | 鲁西化工集团股份有限公司 | System and process for hydrolyzing low-pressure dimethyldichlorosilane |
| CN110694341B (en) * | 2019-10-10 | 2021-09-07 | 唐山三友硅业有限责任公司 | Device and process for treating hydrolysate of hydrogen-containing silicone oil |
| CN111004267A (en) * | 2019-12-13 | 2020-04-14 | 杭州崇耀科技发展有限公司 | Preparation method of hexamethyldisiloxane |
| CN114773230B (en) * | 2022-05-06 | 2024-03-15 | 中国科学院过程工程研究所 | Purifying device and method for methyl polyphenylmethane and polyurethane solution |
| CN114752061B (en) * | 2022-05-27 | 2023-05-30 | 云南能投硅材科技发展有限公司 | Dimethyl dichlorosilane hydrolysis process with desorption function |
| CN114989435B (en) * | 2022-05-29 | 2023-05-30 | 云南能投硅材科技发展有限公司 | Stable control dimethyl dichlorosilane hydrolysis process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090580A (en) * | 1993-02-03 | 1994-08-10 | 化学工业部晨光化工研究院成都分院 | The method for hydrolysis of organic radical silicane dichloride |
| CN101323666B (en) * | 2008-07-24 | 2011-04-27 | 北京石油化工设计院有限公司 | Method for continuous production of hydrolysate by methylchlorosilane concentrated acid hydrolyzing |
-
2013
- 2013-03-28 CN CN201310104637.0A patent/CN103183827B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1090580A (en) * | 1993-02-03 | 1994-08-10 | 化学工业部晨光化工研究院成都分院 | The method for hydrolysis of organic radical silicane dichloride |
| CN101323666B (en) * | 2008-07-24 | 2011-04-27 | 北京石油化工设计院有限公司 | Method for continuous production of hydrolysate by methylchlorosilane concentrated acid hydrolyzing |
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