CN105692554A - Method and equipment for producing high-concentration anhydrous hydrogen chloride methanol solution - Google Patents
Method and equipment for producing high-concentration anhydrous hydrogen chloride methanol solution Download PDFInfo
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- CN105692554A CN105692554A CN201610030436.4A CN201610030436A CN105692554A CN 105692554 A CN105692554 A CN 105692554A CN 201610030436 A CN201610030436 A CN 201610030436A CN 105692554 A CN105692554 A CN 105692554A
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- hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
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Abstract
The invention discloses a method and equipment for producing a high-concentration anhydrous hydrogen chloride methanol solution.The equipment comprises a methanol storage tank, a first-level acid mist filter, a first-level graphite cooler, a second-level acid mist filter, a second-level graphite cooler, a third-level acid mist filter, an enamel stirring tank and a washing tower; the method comprises the steps of firstly, conducting step-by-step acid mist removal and step-by-step cooling on hydrogen chloride gas, then making the hydrogen chloride gas react with methanol, and then washing a product obtained through the reaction.By means of the equipment and method, moisture in the hydrogen chloride gas can be effectively removed, the concentration of the hydrogen chloride methanol solution can be improved, consumption of the methanol solution is reduced, and thereby the problems that production cost and sale price are generally higher due to the fact that existing methanol hydrogen chloride solutions are low in concentration, high in water content and large in consumption are solved.
Description
Technical field
The invention belongs to industrial chemicals preparation field, especially relate to a kind of method and apparatus producing high concentration anhydrous hydrogen chloride methanol solution。
Background technology
Under hydrogen chloride normal pressure colourless, fusing point-114.2 spend, boiling point-85 spend, there is asphyxiant abnormal smells from the patient, upper respiratory tract is had strong stimulation, eye, skin, mucosa are had corrosion, it is a kind of conventional Inorganic Chemicals, is widely used in the industries such as dyestuff, pesticide, medicine, food, dyestuff, leather, metallurgy。
The technique producing hydrogen chloride at present has: (1) electrolysis NaCl generates H2 and Cl2, is lighted by hydrogen, then pass to chlorine and react in synthetic furnace, prepares hydrogen chloride gas;(2) NaCl or CaCl2 adds sulphuric acid and generate hydrogen chloride gas, through remove impurity, after drying prepared hydrogen chloride gas。
Hydrogen chloride gas is a kind of gas being difficult to and compressing and liquefying, and if desired uses anhydrous hydrogen chloride gas to build device or buy absolute methanol hydrogen chloride solution。Wherein, build hydrogen chloride installation cost higher, and to the another fixed pollution of environment, therefore a lot of parties in request select to use methanolic hydrogen chloride solution extracting directly anhydrous hydrogen chloride solution。But through the investigation in methanol-hydrogen chloride market is found, owing to industrialized production hydrogen chloride gas contains more moisture, conventional dewatering such as concentrated sulphuric acid dries to dry etc. with anhydrous CaCl2 and is very difficult to remove the moisture in hydrogen chloride gas, the sale concentration making current methanolic hydrogen chloride solution is typically between 18%~25%, between moisture 1%~5%, namely methanolic hydrogen chloride solution concentration is relatively low, moisture higher, thus it is very big to result in the amount needing methanol solution, price plus methanol solution itself is higher so that production cost and selling price are generally higher。
Summary of the invention
The present invention provides a kind of method and apparatus producing high concentration anhydrous hydrogen chloride methanol solution, the method and equipment can effectively remove the moisture content in hydrogen chloride gas, improves the concentration of hydrogen chloride methanol solution, reduce the consumption of methanol solution, thus solving the production cost that causes because of existing methanolic hydrogen chloride solution concentration higher, methanol solution large usage quantity low, moisture and the generally higher problem of selling price。
In order to solve above-mentioned technical problem, one of the technical solution used in the present invention is:
It includes methanol storage tank, enamel stirred tank and water scrubber;The methanol outlet of described methanol storage tank is connected with the methanol solution import of enamel stirred tank, and the methanol of described enamel stirred tank-hydrogen chloride outlet is connected with the methanol-hydrogen chloride import of water scrubber;The hydrogen chloride import of described enamel stirred tank is connected by the hydrogen chloride outlet of three grades of acid mist filters and two grades of graphite coolers, the hydrogen chloride import of described two grades of graphite coolers is connected with the hydrogen chloride outlet of one-level graphite cooler by two grades of acid mist filters, and the hydrogen chloride import of described one-level graphite cooler is connected to primary acids mist resistant filter。
In technique scheme, technical scheme is more specifically: be provided with graphite ejector between described three grades of acid mist filters and the hydrogen chloride import of described enamel stirred tank;It is externally provided with cooling jacket at described enamel stirred tank。
Further, described primary acids mist resistant filter, described two grades of acid mist filters and described three grades of acid mist filters are all that the glass fibre adopting dipping hydrophobicity fluorine containing silicone oil is made。
Another technical scheme of the present invention is:
Adopting a kind of equipment producing high concentration anhydrous hydrogen chloride methanol solution, this equipment includes methanol storage tank, enamel stirred tank and water scrubber;The methanol outlet of described methanol storage tank is connected with the methanol solution import of enamel stirred tank, and the methanol of described enamel stirred tank-hydrogen chloride outlet is connected with the methanol-hydrogen chloride import of water scrubber;The hydrogen chloride import of described enamel stirred tank is connected by the hydrogen chloride outlet of three grades of acid mist filters and two grades of graphite coolers, the hydrogen chloride import of described two grades of graphite coolers is connected with the hydrogen chloride outlet of one-level graphite cooler by two grades of acid mist filters, and the hydrogen chloride import of described one-level graphite cooler is connected to primary acids mist resistant filter;It is provided with graphite ejector between described three grades of acid mist filters and the hydrogen chloride import of described enamel stirred tank;It is externally provided with cooling jacket at described enamel stirred tank;Described primary acids mist resistant filter, described two grades of acid mist filters and described three grades of acid mist filters are all that the glass fibre adopting dipping hydrophobicity fluorine containing silicone oil is made;
The method includes step in detail below:
A, by hydrogen chloride gas with 200m3/ h~300m3The flow velocity of/h enters in primary acids mist resistant filter, removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of B, step A enters in one-level graphite cooler, and precools at 5 DEG C~7 DEG C;
Hydrogen chloride gas after C, B process enters in two grades of acid mist filters, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of D, step C enters in two grades of graphite coolers, and cools down at-35 DEG C~-20 DEG C;
Hydrogen chloride gas after E, D step process enters in three grades of acid mist filters, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after F, E step process enters in enamel stirred tank, simultaneously by the methanol in methanol storage tank with 3m3/ h~5m3The flow velocity of/h enters in enamel stirred tank, and makes hydrogen chloride gas and methanol at-5 DEG C~80 DEG C, stirring reaction 4h~6h;
Product that G, F step reaction obtains enters in water scrubber, 30 DEG C~60 DEG C, washing under normal pressure。
Adopt technique scheme, obtain providing the benefit that:
1. the present invention produces high concentration anhydrous hydrogen chloride methanol solution to provide the equipment of necessity, especially the path being sequentially connected with composition of primary acids mist resistant filter 2, one-level graphite cooler 3, two grades of acid mist filters, 5 three grades of acid mist filters 6 of 4, two grades of graphite coolers, can effectively remove the moisture content that raw material hydrogen chloride gas contains, its water content is made to reach minima, so that itself and methanol solution are finally made high concentration anhydrous hydrogen chloride methanol solution。
2. the graphite ejector arranged between the hydrogen chloride import on three grades of acid mist filters and enamel stirred tank top can effectively improve the injection flow velocity of methanol, it is speed energy by pressure energy, make the low generation vacuum of air-breathing district Pressure Drop, accelerate the mixing velocity of hydrogen chloride gas and methanol。
3. the present invention is provided with cooling jacket at enamel stirred tank outer surface, it is possible to make hydrogen chloride gas and methanol cool down more uniform at enamel stirred tank whipping process, mixing more thorough。
4. due in raw material hydrogen chloride gas lyophilization dry run, the hydrochloric acid of about the 40% of condensation, except be on a small quantity with shaped liquid film from graphite cooler tubulation inwalls at different levels flow out except, major part is suspended in air-flow in atomic thin " acid mist ", formed " aerosol ", therefore, the acid mist filter that the present invention makes by adopting the glass fibre of dipping hydrophobicity fluorine containing silicone oil, the glass fibre making " aerosol " vertical with acid mist filter collides, thus major part droplet in retaining down " aerosol ", then in the process that the power of relying on for support flows downward, drop is gradually increased again, finally drop down and discharge, thus the water content reduced in hydrogen chloride gas。
5. the present invention utilizes the hygroscopicity of hydrogen chloride, is precipitated out with the hydrochloric acid mist of about 40% by moisture content in raw material hydrogen chloride gas at a lower temperature, reaches the purpose of raw material hydrogen chloride gas dehydrate;Then, the raw material hydrogen chloride gas after this dehydrate and methanol prepare product hydrogen chloride methanol solution within specified temperatures, and in this hydrogen chloride methanol solution, the dissolubility of hydrogen chloride is up to 50%~55%, and its water content is low to moderate 20ppm~80ppm。
6. although the water content of raw material hydrogen chloride gas depends on the vapor partial pressure on about 40% hydrochloric acid solution at this temperature, namely mixture temperature is more low, water content is also more little, but if the too low concentrated hydrochloric acid of temperature can precipitate out the crystallization of HCl 2H2O, cause the blocking of pipeline, therefore the present invention is by being limited in specific scope the chilling temperature of coolers at different levels, is possible not only to make the water content of raw material hydrogen chloride gas reach minimum, it is also possible to guarantee the unobstructed of its pipeline。
Accompanying drawing explanation
Fig. 1 is the structural representation that the present invention produces the equipment of high concentration anhydrous hydrogen chloride methanol solution。
Specific embodiment
Below in conjunction with accompanying drawing, the invention will be further described:
Embodiment 1
Shown in Fig. 1 is the structure chart of the equipment producing high concentration anhydrous hydrogen chloride methanol solution, including methanol storage tank 1, primary acids mist resistant filter 2,3, two grades of acid mist filters of one-level graphite cooler, 5, three grades of acid mist filters 6 of 4, two grades of graphite coolers, enamel stirred tank 7 and water scrubber 8;The methanol outlet 9 of methanol storage tank 1 lower end is connected with the methanol solution import 10 on enamel stirred tank 7 top;The hydrogen chloride outlet 11 of primary acids mist resistant filter 2 is connected with the hydrogen chloride import 12 on one-level graphite cooler 3 top, the hydrogen chloride outlet 13 of one-level graphite cooler 3 lower end is connected with the hydrogen chloride import 14 of two grades of acid mist filters 4, the hydrogen chloride outlet 15 of two grades of acid mist filters 4 is connected with the hydrogen chloride import 16 on two grades of graphite cooler 5 tops, the hydrogen chloride outlet 17 of two grades of graphite cooler 5 lower ends is connected with the hydrogen chloride import 18 of three grades of acid mist filters 6, and the hydrogen chloride outlet 19 of three grades of acid mist filters 6 is connected with the hydrogen chloride import 20 on enamel stirred tank 7 top;The methanol on enamel stirred tank 7 top-hydrogen chloride outlet 21 is connected with the methanol-hydrogen chloride import 22 of water scrubber 8 lower end;Being provided with graphite ejector 23 between the hydrogen chloride import 20 on three grades of acid mist filters 6 and described enamel stirred tank 7 top, enamel stirred tank 7 outer surface is provided with cooling jacket 24;1, two grades of acid mist filters 4 of primary acids mist resistant filter and three grades of acid mist filters 6 are all that the glass fibre adopting dipping hydrophobicity fluorine containing silicone oil is made。
The present embodiment is produce high concentration anhydrous hydrogen chloride methanol solution to provide the equipment of necessity, especially the path being sequentially connected with composition of primary acids mist resistant filter 2, one-level graphite cooler 3, two grades of acid mist filters, 5 three grades of acid mist filters 6 of 4, two grades of graphite coolers, can effectively remove the moisture content that raw material hydrogen chloride gas contains, its water content is made to reach minima, so that itself and methanol solution are finally made high concentration anhydrous hydrogen chloride methanol solution。
Embodiment 2
The equipment that the present embodiment adopts includes methanol storage tank 1, primary acids mist resistant filter 2,3, two grades of acid mist filters of one-level graphite cooler, 5, three grades of acid mist filters 6 of 4, two grades of graphite coolers, enamel stirred tank 7 and water scrubber 8;The methanol outlet 9 of methanol storage tank 1 lower end is connected with the methanol solution import 10 on enamel stirred tank 7 top;The hydrogen chloride outlet 11 of primary acids mist resistant filter 2 is connected with the hydrogen chloride import 12 on one-level graphite cooler 3 top, the hydrogen chloride outlet 13 of one-level graphite cooler 3 lower end is connected with the hydrogen chloride import 14 of two grades of acid mist filters 4, the hydrogen chloride outlet 15 of two grades of acid mist filters 4 is connected with the hydrogen chloride import 16 on two grades of graphite cooler 5 tops, the hydrogen chloride outlet 17 of two grades of graphite cooler 5 lower ends is connected with the hydrogen chloride import 18 of three grades of acid mist filters 6, and the hydrogen chloride outlet 19 of three grades of acid mist filters 6 is connected with the hydrogen chloride import 20 on enamel stirred tank 7 top;The methanol on enamel stirred tank 7 top-hydrogen chloride outlet 21 is connected with the methanol-hydrogen chloride import 22 of water scrubber 8 lower end;Being provided with graphite ejector 23 between the hydrogen chloride import 20 on three grades of acid mist filters 6 and described enamel stirred tank 7 top, enamel stirred tank 7 outer surface is provided with cooling jacket 24;1, two grades of acid mist filters 4 of primary acids mist resistant filter and three grades of acid mist filters 6 are all that the glass fibre adopting dipping hydrophobicity fluorine containing silicone oil is made
Its concrete production process is as follows:
A, by hydrogen chloride gas with 200m3The flow velocity of/h enters in primary acids mist resistant filter 2, removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of B, step A enters in one-level graphite cooler 3, and precools at 5 DEG C;
Hydrogen chloride gas after C, B process enters in two grades of acid mist filters 4, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of D, step C enters in two grades of graphite coolers 5, and cools down at-35 DEG C;
Hydrogen chloride gas after E, D step process enters in three grades of acid mist filters 6, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after F, E step process enters in enamel stirred tank 7, simultaneously by the methanol in methanol storage tank 1 with 3m3The flow velocity of/h enters in enamel stirred tank 7, and makes hydrogen chloride gas and methanol at-5 DEG C, stirring reaction 4h;
Product that G, F step reaction obtains enters in water scrubber, 30 DEG C, washing under normal pressure。
In the product hydrogen chloride methanol solution that the present embodiment 1 prepares, the dissolubility of hydrogen chloride is up to 55%, and its water content is low to moderate 20ppm。
Embodiment 3
The present embodiment produces structure such as embodiment 1 of the equipment that high concentration anhydrous hydrogen chloride methanol solution adopts;
Its concrete production process is as follows:
A, by hydrogen chloride gas with 250m3The flow velocity of/hh enters in primary acids mist resistant filter 1, removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of B, step A enters in one-level graphite cooler (3), and precools at 6 DEG C;
Hydrogen chloride gas after C, B process enters in two grades of acid mist filters 4, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of D, step C enters in two grades of graphite coolers 5, and cools down at-28 DEG C;
Hydrogen chloride gas after E, D step process enters in three grades of acid mist filters 6, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after F, E step process enters in enamel stirred tank 7, simultaneously by the methanol in methanol storage tank 1 with 4m3The flow velocity of/h enters in enamel stirred tank 7, and makes hydrogen chloride gas and methanol at 0 DEG C, stirring reaction 5h;
Product that G, F step reaction obtains enters in water scrubber, 40 DEG C, washing under normal pressure。
In the product hydrogen chloride methanol solution that the present embodiment 2 prepares, the dissolubility of hydrogen chloride is up to 53%, and its water content is low to moderate 40ppm。
Embodiment 4
The present embodiment produces structure such as embodiment 1 of the equipment that high concentration anhydrous hydrogen chloride methanol solution adopts;
Its concrete production process is as follows:
A, by hydrogen chloride gas with 300m3The flow velocity of/h enters in primary acids mist resistant filter 1, removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of B, step A enters in one-level graphite cooler 3, and precools at 7 DEG C;
Hydrogen chloride gas after C, B process enters in two grades of acid mist filters 4, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of D, step C enters in two grades of graphite coolers 5, and cools down at-20 DEG C;
Hydrogen chloride gas after E, D step process enters in three grades of acid mist filters 6, again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after F, E step process enters in enamel stirred tank 7, simultaneously by the methanol in methanol storage tank 1 with 5m3The flow velocity of/h enters in enamel stirred tank 7, and makes hydrogen chloride gas and methanol at 5 DEG C, stirring reaction 6h;
Product that G, F step reaction obtains enters in water scrubber, 60 DEG C, washing under normal pressure。
In the product hydrogen chloride methanol solution that the present embodiment 3 prepares, the dissolubility of hydrogen chloride is up to 50%, and its water content is low to moderate 60ppm。
Claims (4)
1. the equipment producing high concentration anhydrous hydrogen chloride methanol solution, include methanol storage tank (1), enamel stirred tank (7) and water scrubber (8), it is characterized in that: the methanol outlet (9) of described methanol storage tank (1) is connected with the methanol solution import (10) of enamel stirred tank (7), the methanol of described enamel stirred tank (7)-hydrogen chloride outlet (21) is connected with the methanol-hydrogen chloride import (22) of water scrubber (8);The hydrogen chloride import (20) of described enamel stirred tank (7) exports (17) by three grades of acid mist filters (6) with the hydrogen chloride of two grades of graphite coolers (5) and is connected, the hydrogen chloride import (16) of described two grades of graphite coolers (5) exports (13) by two grades of acid mist filters (4) with the hydrogen chloride of one-level graphite cooler (3) and is connected, and the hydrogen chloride import (12) of described one-level graphite cooler (3) is connected to primary acids mist resistant filter (2)。
2. the equipment of production high concentration anhydrous hydrogen chloride methanol solution according to claim 1, it is characterised in that: between described three grades of acid mist filters (6) and the hydrogen chloride import (20) of described enamel stirred tank (7), it is provided with graphite ejector (23);It is externally provided with cooling jacket (24) described enamel stirred tank (7)。
3. the equipment of production high concentration anhydrous hydrogen chloride methanol solution according to claim 1 and 2, it is characterised in that: described primary acids mist resistant filter (1), described two grades of acid mist filters (4) and described three grades of acid mist filters (6) they are all that the glass fibre adopting dipping hydrophobicity fluorine containing silicone oil is made。
4. the method producing high concentration anhydrous hydrogen chloride methanol solution, it is characterised in that: adopting a kind of equipment producing high concentration anhydrous hydrogen chloride methanol solution, this equipment includes methanol storage tank (1), enamel stirred tank (7) and water scrubber (8);The methanol outlet (9) of described methanol storage tank (1) is connected with the methanol solution import (10) of enamel stirred tank (7), and the methanol of described enamel stirred tank (7)-hydrogen chloride outlet (21) is connected with the methanol-hydrogen chloride import (22) of water scrubber (8);The hydrogen chloride import (20) of described enamel stirred tank (7) exports (17) by three grades of acid mist filters (6) with the hydrogen chloride of two grades of graphite coolers (5) and is connected, the hydrogen chloride import (16) of described two grades of graphite coolers (5) exports (13) by two grades of acid mist filters (4) with the hydrogen chloride of one-level graphite cooler (3) and is connected, and the hydrogen chloride import (12) of described one-level graphite cooler (3) is connected to primary acids mist resistant filter (2);It is provided with graphite ejector (23) between described three grades of acid mist filters (6) and the hydrogen chloride import (20) of described enamel stirred tank (7);It is externally provided with cooling jacket (24) described enamel stirred tank (7);Described primary acids mist resistant filter (1), described two grades of acid mist filters (4) and described three grades of acid mist filters (6) are all that the glass fibre adopting dipping hydrophobicity fluorine containing silicone oil is made;
The method includes step in detail below:
A, by hydrogen chloride gas with 200m3/ h~300m3The flow velocity of/h enters in primary acids mist resistant filter (2), removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of B, step A enters in one-level graphite cooler (3), and precools at 5 DEG C~7 DEG C;
Hydrogen chloride gas after C, B process enters in two grades of acid mist filters (4), again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after the process of D, step C enters in two grades of graphite coolers (5), and cools down at-35 DEG C~-20 DEG C;
Hydrogen chloride gas after E, D step process enters in three grades of acid mist filters (6), again removes the acid mist contained in hydrogen chloride gas;
Hydrogen chloride gas after F, E step process enters in enamel stirred tank (7), simultaneously by the methanol in methanol storage tank (1) with 3m3/ h~5m3The flow velocity of/h enters in enamel stirred tank (7), and makes hydrogen chloride gas and methanol at-5 DEG C~80 DEG C, stirring reaction 4h~6h;
Product that G, F step reaction obtains enters in water scrubber (8), 30 DEG C~60 DEG C, washing under normal pressure。
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CN201610030436.4A CN105692554A (en) | 2016-01-18 | 2016-01-18 | Method and equipment for producing high-concentration anhydrous hydrogen chloride methanol solution |
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Cited By (2)
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CN108837667A (en) * | 2018-06-27 | 2018-11-20 | 青岛科技大学 | A kind of absorption of hydrogen chloride gas and its desorption method and application |
CN108929191A (en) * | 2018-06-28 | 2018-12-04 | 湖北兴瑞硅材料有限公司 | The technique and device of methylchlorosilane hydrolysis hydrogen chloride synthesis chloromethanes |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108837667A (en) * | 2018-06-27 | 2018-11-20 | 青岛科技大学 | A kind of absorption of hydrogen chloride gas and its desorption method and application |
CN108929191A (en) * | 2018-06-28 | 2018-12-04 | 湖北兴瑞硅材料有限公司 | The technique and device of methylchlorosilane hydrolysis hydrogen chloride synthesis chloromethanes |
CN108929191B (en) * | 2018-06-28 | 2021-02-02 | 湖北兴瑞硅材料有限公司 | Process and device for synthesizing chloromethane by hydrolyzing hydrogen chloride with methylchlorosilane |
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