CN101781181A - Method of preparing chloropinacolone by gas-phase photocatalysis chlorination and special device thereof - Google Patents
Method of preparing chloropinacolone by gas-phase photocatalysis chlorination and special device thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of chloropinacolone and a special device thereof. The method comprises the following steps: pinacolone is adopted as a raw material inside a chlorination reaction device and has chlorination reaction with the chlorination gas under the radiation of the light source to obtain the chloropinacolone, the chlorination reaction device comprises a reaction kettle with a heating device, a rectifying column which is arranged above an outlet of the reaction kettle, a gas-phase reactor which is arranged at a chlorination gas access inlet and a condenser, and also comprises a gas-liquid separator and a backflow liquid sealing pipe; and in the reaction kettle, the rectifying raw material gas and the chlorination gas or the chlorination mixed gas are undertaken the gas-phase photocatalysis chlorination reaction inside a gas-phase reactor from top to bottom to generate the chloropinacolone.The method is not only simple and easy, is easy to be industrialized, has low cost, less side product and high conversion rate and can prepare the chloropinacolone with high content, but also the special device for preparing the chloropinacolone is applicable to the industrialized production.
Description
(1) technical field
The present invention relates to the preparation method and the isolated plant thereof of a chloropinacolone.
(2) background technology
One chloropinacolone is important agricultural chemicals, medicine intermediate, is made by the pinacolone direct chlorination usually.
Present industrial production one chloropinacolone adopts the low-temperature solvent method more, has reported " the synthetic and application of a chlorine pinacolone " [" Henan chemical industry ", 06,1993] as people such as Zhang Weimins, makes the solvent cut pinacolone with methyl alcohol, or uses N
2Gas dilution Cl
2Gas is being lower than chlorination under 0 ℃ the low temperature, to reduce the production rate of two chloropinacolones; But limit by raw material and processing condition, product purity has only about 90% usually, and two chloropinacolone content are up to 7%, because two chloropinacolones and a chloropinacolone boiling point only differ 0.6 ℃, and character is close, is difficult to separate from product, can not get a highly purified chloropinacolone.Such quality product directly influences the production of agricultural chemicals, pharmaceutical prod.As report such as Gao Chengshun " improving the superficial view of triazolone yield, quality " [" agricultural chemicals ", 02,1990] in agricultural chemicals triazolone synthetic, two chloropinacolones can and raw material P-Chlorophenol, intermediate ether ketone generation side reaction, cause the triazolone quality to reduce, yield decline.And improve the key of triazolone quality and yield, and to improve the quality of a chloropinacolone exactly, make it to contain less two chloropinacolones.Pinacolone and Cl
2Air exhaustion easily reacts, and also can spontaneously carry out even react under 0 ℃ of low temperature.Chlorination reaction is a strong exothermal reaction, and the low-temperature solvent method is to adopt the batch still operation, and logical-15 ℃ of refrigerated waters of chuck also difficulty in time shift out exothermic heat of reaction, only restricted logical chlorine speed is come control reaction temperature, so the production cycle is long, and equipment capacity is low, and process is wayward.For overcoming above-mentioned drawback, Shen Bo etc. report " tubular reactor synthesizes a chloropinacolone technical study " [" chemical reaction engineering and technology ", 14 (1), 1998] adopt tubular reactor to carry out the chlorination reaction of pinacolone, utilize the less back-mixing feature of tubular reactor, under suitable condition, suppress the chlorination of the pinacolone degree of depth effectively.Simultaneously the tubular reactor reaction member is little, and the unit reaction volume has bigger heat-transfer surface, and heat passage by tube wall has higher heat transfer efficiency.Exothermic heat of reaction can be got rid of rapidly, and process temperature is easy to control; But the content of two chloropinacolones still surpasses 2.3% in the product that obtains, and polychloride impurity such as the raw materials cost of the derived product of failing to solve well, two chloropinacolones are to the quality influence of derived product and to the pollution problem of environment.
When the contriver studies in this area, design a kind of new gas-phase photocatalysis and prepared the method for a chloropinacolone, and designed the pinacolone monochlor(in)ate reaction unit of novel special use.
(3) summary of the invention
Purpose of the present invention just provides the method and apparatus of a kind of simple and easy to do, easy industrialization, cost is low, by product is few, transformation efficiency is higher preparation one chloropinacolone.
The technical solution used in the present invention is as follows:
A kind of pinacolone gas-phase photocatalysis chlorination prepares the method for a chloropinacolone, described method is to be raw material with the pinacolone in chlorination reaction device, under rayed, make a chloropinacolone with chloridating gas generation chlorination reaction, described chlorination reaction device comprises the reactor that has heating unit, be located at the rectifying column of reactor outlet top, be provided with the Gas-phase reactor that chloridating gas feeds mouth, condenser, described chlorination reaction device also comprises gas-liquid separator and phegma tube sealing, described reactor pass-out mouth top connects rectifying column, rectifying column is suitable for reading to be connected with Gas-phase reactor by folding shape pipe, described Gas-phase reactor is that inlet mouth is located at the top and is with temperature measuring equipment, outlet is located at below and vertically arranged transparent unit, here with folding shape pipe rectifying column is connected with Gas-phase reactor, when main reaction, when making the airflow passes Gas-phase reactor, air flow line from top to bottom, the inlet of Gas-phase reactor is located at the top and is with temperature measuring equipment during installation, outlet is located at the below, the air flow line that guarantees reaction is from top to bottom, described Gas-phase reactor periphery is provided with light source light according to device, described chloridating gas feeds the top that mouth is located at Gas-phase reactor, air flow line is vertically downward in the described Gas-phase reactor when guaranteeing chlorination reaction, described condenser one end and Gas-phase reactor outlet are joined, the other end connects gas-liquid separator, described gas-liquid separator output terminal comprises pneumatic outlet and liquid exit, described liquid exit communicates with rectifying column bottom or reactor upper interface by the phegma tube sealing, guarantee that withdrawing fluid enters reactor, described reactor, rectifying column, adjustable pipe, folding shape pipe, Gas-phase reactor, condenser, gas-liquid separator and phegma tube sealing are communicated with the circulation line that constitutes reaction system successively.Light source of the present invention comprises natural light, fluorescent lamp and ultra-violet lamp.
Further described method is: drop into pinacolone in reactor, inject a little raw material in the phegma tube sealing, reaching the fluid-tight effect is that gas can not pass through, open the heating unit of reactor, reflux, treat that Gas-phase reactor temperature in (T2) reaches near raw material boiling temperature (than low 2 ℃ of raw material boiling point), and when the condenser outlet at bottom has backflow, slowly open the chloridating gas intake valve, under light source irradiation by the reactor heating and gasifying generate pinacolone and chloridating gas generation chlorination reaction generate a chloropinacolone, by condenser condenses air inlet liquid/gas separator is arranged simultaneously, it is acid that tail gas is, control reactor rate of heating and chlorine feeding amount keep stable and reflux; Along with the reaction continue carry out, reactor temperature (T1) can continue to rise, when the question response temperature in the kettle reaches in 130 ℃～160 ℃ scopes, stop logical chloridating gas, product evaporates under normal pressure removes raw material, residuum is mainly a chloropinacolone, and described chloridating gas is the mixed gas of the arbitrary proportion of chlorine or chlorine and rare gas element, and described rare gas element is nitrogen, helium or argon gas.
A kind of isolated plant that is used for the preparation of the present invention's one chloropinacolone, described isolated plant comprises the reactor of being with well heater, be located at the rectifying column of reactor outlet top, be provided with the Gas-phase reactor that chloridating gas feeds mouth, condenser, described chlorination reaction device also comprises gas-liquid separator and phegma tube sealing, described rectifying column is connected with Gas-phase reactor by folding shape pipeline, described Gas-phase reactor is located at the top for inlet, outlet is located at below and vertically arranged transparent unit, described Gas-phase reactor periphery is provided with light source light according to device, described chloridating gas feeds the top that mouth is located at Gas-phase reactor, described upper end of condenser and Gas-phase reactor outlet are joined, the other end connects gas-liquid separator, described gas-liquid separator output terminal is pneumatic outlet and liquid exit, described liquid exit communicates described reactor by the phegma tube sealing with rectifying column bottom or reactor upper interface, rectifying column, adjustable pipe, folding shape pipeline, Gas-phase reactor, condenser, gas-liquid separator, the phegma tube sealing, rectifying column bottom or reactor upper interface communicate and are communicated with the circulation line that constitutes reaction system successively.
Reaction among the present invention is to carry out under natural light or daylight light or UV-irradiation, and the raw material that relates among the present invention is a pinacolone, and structure is:
Product one chloropinacolone is:
By product two chloropinacolones are:
The used chloridating gas of the present invention can be that chlorine also can be the mixed gas of chlorine and rare gas element, and rare gas element can be nitrogen, helium, argon gas etc., and rare gas element accounts for the ratio of chloridating gas and is advisable at 0-80%, is preferably between the 20-50%; Usually the amount of the chloridating gas of rate of heating that the amount of pinacolone unstripped gas can be by raw material in the reactor and input is controlled.
Further, the outside surface of described Gas-phase reactor is provided with the optical throughput setter of may command illumination.Optical throughput setter as described is telescopic darkening ring.Stretch up and down by shading figure and to regulate the quantity of illumination that Gas-phase reactor is subjected to, thus the control reaction process.
Further more described folding shape pipeline is one " n " font pipeline, and an end and rectifying column are tightly connected, and the other end connects that chloridating gas feeds mouthful and is tightly connected with the Gas-phase reactor upper end and forms.For the convenience of installing, described folding shape pipeline also can be connected with rectifying column by corrugated tube.
Further, described phegma tube sealing is a U-shaped pipe, and the level attitude of the end that described U-shaped pipe is connected with gas-liquid separator is higher than the other end that is connected with rectifying column bottom or reactor upper interface.
Gas-liquid separator pneumatic outlet of the present invention is connected with the hydrogen chloride absorption device.
Isolated plant of the present invention, along with the carrying out of reaction, an increasing chloropinacolone is got back to reactor, and the temperature in the reactor constantly raises, and when being elevated to than a chloropinacolone boiling point in low 10 ℃～50 ℃ scopes, just finishes reaction.
Concrete, isolated plant of the present invention, comprise the reactor of being with heating unit, be located at reactor and export the rectifying column (1) that the top has thermal insulation layer, regulate rectifying column and the adjustable pipe (2) of rolling over shape pipeline fit-up gap, the folding shape pipe (3) of chloridating gas inlet pipe (10) can be installed, be provided with the Gas-phase reactor (4) that chloridating gas feeds mouth, the Gas-phase reactor periphery is provided with the telescopic darkening ring (5) of may command illumination, condenser (6), gas-liquid separator (7), phegma tube sealing (8) and light source (9), a described chloropinacolone prepares isolated plant and is connected with reactor with the gas-liquid separator liquid exit by rectifying column end opening or rectifying column end opening, described rectifying column (1) is by adjustable pipe (2), the folding shape pipe (3) of " n " font is connected with the inlet mouth of Gas-phase reactor (4), described inlet pipe (10) is installed in folding shape pipe (3) and the vertical pipeline section that Gas-phase reactor (4) links to each other, described Gas-phase reactor is located at the top for inlet, the transparent unit that outlet is located at the below and vertically installs, the material of described Gas-phase reactor is recommended as colourless transparent glass or quartzy material, described Gas-phase reactor periphery is provided with the telescopic darkening ring of optical throughput setter (5) of may command illumination, described chloridating gas feeds the top that mouth is located at Gas-phase reactor, described condenser one end and Gas-phase reactor outlet are joined, the condenser the other end connects gas-liquid separator, described gas-liquid separator output terminal is the pneumatic outlet that makes progress of opening and the liquid exit that Open Side Down, described liquid exit communicates with rectifying column bottom or reactor upper interface by the phegma tube sealing, described phegma tube sealing is a U-shaped pipe, the end level attitude that described U-shaped pipe is connected with gas-liquid separator (7) is higher than the other end that is connected with rectifying column bottom or reactor upper interface, an end that is connected with rectifying column bottom or reactor upper interface is the level of state described reactor, rectifying column, adjustable pipe, folding shape pipe, Gas-phase reactor, condenser, gas-liquid separator, the phegma tube sealing, rectifying column bottom or reactor upper interface seal successively and are communicated with the circulation line that constitutes reaction system.
Photochemical catalysis gas phase optical chlorinating reaction device of the present invention is a kind of special reaction unit, it is glass, lass lining or enamel that rectifying column is recommended material, it is tetrafluoroethylene that adjustable pipe is recommended material, and the material of inlet pipe is recommended as tetrafluoroethylene, glass, lass lining or enamel; The material of Gas-phase reactor is recommended as transparent glass, quartz, optical throughput setter material is recommended as metal or other antiultraviolet material, condenser, gas-liquid separator, phegma pipe sealing material can be glass, lass lining or enamel, and light source can be natural light, daylight light or UV-light.Adjustable pipe adopts usually certain elastic corrugated tube, and as the corrugated tube of polytetrafluoroethylmaterial material preparation, reaction times among the present invention and temperature are determined according to reaction raw materials and reactor size.
The singularity of this reactor is that gas-phase reaction carried out by top downwards, be that rectifying unstripped gas and chloridating gas or chlorination gas mixture pass through the photocatalysis chlorination reactor from top to bottom in the reactor in Gas-phase reactor, lower greatly or when having avoided gas-phase reaction from bottom to top by reactor resultant contact the generation polychloride again with chlorine.As everyone knows, the product boiling point after the raw material chloro is higher than 106 ℃ of raw material boiling points for 172 ℃, understands in reactor under the condensation; When if the reaction mixture gas body passes through reactor from bottom to top, the chloro thing boiling point that the catalyzed reaction of light chlorination faster generates is higher than hybrid reaction gas and condensation is got off, but because reactant gases constantly moves upward, one chloro thing condensation lowering speed can slow down, even be suspended in the reactant gases, increased the duration of contact with chlorine, further the chlorating probability increases greatly, polychloride content increase in the product causes by product to increase in the end reaction still; Method of the present invention has solved this problem well, and polychloride is significantly reduced.
According to the reaction gas flow size, regulate the optical throughput setter, increase or reduce plane of illumination, can regulate the chlorination reaction progress; Can be equipped with 1-5 this device according to the reactor size simultaneously.
By the present invention, can obtain a chloropinacolone and prepare isolated plant; Utilize gas-phase photocatalysis chlorination reaction of the present invention, be equipped with this device on reactor or rectifying still, can make high-content one chloropinacolone product, its operational condition and physical parameter are as shown in table 1.
The described reactor of apparatus of the present invention can be a rectifying still also, during reaction, is that inert gas tube and chlorine tube and inlet pipe are joined with chloridating gas, and the pneumatic outlet of gas-liquid separator connects the hydrogen chloride absorption device, the total system nitrogen replacement; Pinacolone is added reactor, inject a little pinacolone blocking-up gas in the phegma tube sealing and pass through, reactor begins heating, after the raw material boiling, raw material vapor enters Gas-phase reactor through rectifying column, adjustable pipe, folding shape pipe, enters gas-liquid separator after continuing to flow to condenser; Select suitable light source, after flow of feed gas is stable, when the Gas-phase reactor temperature in reaches near the raw material boiling temperature, open the inlet pipe valve, this moment, reaction was carried out at once, carry out optical chlorinating reaction in the Gas-phase reactor from top to down, the chloropinacolone, hydrogenchloride and the unreacting material that generate, immediately along air flow line downwards through condenser condenses, raw material, a chloropinacolone are separated with the hydrogenchloride of generation through gas-liquid separator, hydrogenchloride removes absorption unit, raw material, a chloropinacolone flow into reactor through the phegma tube sealing, so circulation; As long as control reactor rate of heating, chloridating gas flow, plane of illumination and select suitable light source well, just can guarantee that it is a chloropinacolone that raw material more than 90% is chlorinated, and have only many chloro-products of minute quantity, the reuse of pressure reducing and steaming raw material, the still liquid that obtains is without rectifying, one chloropinacolone content just can reach more than 99.5%. and the polychloride amount is few, meets the requirement of cleaner production, green production process, has significantly reduced generation of waste.
Method of the present invention is not only the method for a kind of simple and easy to do, easy industrialization, cost is low, by product is few, transformation efficiency is higher preparation one chloropinacolone, and a chloropinacolone of invention prepares isolated plant and is fit to suitability for industrialized production.
Table 1 raw material and product structure, physical parameter and photochemical catalysis gas phase chlorination reaction table look-up
(4) description of drawings
Fig. 1 is used for preparing the isolated plant of a chloropinacolone for the present invention, among the figure
The 1--rectifying column; The 2--adjustable pipe; 3-folding shape pipe; The 4-Gas-phase reactor; The telescopic darkening ring of 5-; The 6-condenser; The 7-gas-liquid separator; 8-phegma tube sealing; 9-illumination light source; The 10-inlet pipe.
(5) embodiment:
Below with specific embodiment technical scheme of the present invention is described, but protection scope of the present invention is not limited thereto:
Embodiment 1 isolated plant concrete structure of the present invention is as follows:
A kind of isolated plant that is used for preparing a chloropinacolone, comprise reactor, the rectifying column (1) (enamel material) that has thermal insulation layer, regulate the adjustable pipe (2) (tetrafluoroethylene material) of rectifying column and folding shape pipe fit-up gap, can be installed into folding shape pipe (3) (enamel material) of tracheae (10) (glass material), be provided with the Gas-phase reactor (4) (transparent glass material) that chloridating gas feeds mouth, the Gas-phase reactor periphery is provided with the telescopic darkening ring of optical throughput setter (5) (iron sheet material) of may command illumination, condenser (6) (enamel material), gas-liquid separator (7) (glass material), phegma tube sealing (8) (glass material) and fluorescent light source (9), a described chloropinacolone prepares isolated plant, the rectifying column end opening is connected with reactor, described rectifying column (1) is by adjustable pipe (2), the folding shape pipe (3) of " n " shape is connected with the inlet mouth of Gas-phase reactor (4), described inlet pipe (10) is installed in folding shape pipe (3) and the vertical pipeline section that Gas-phase reactor (4) links to each other, described Gas-phase reactor is located at the top for inlet, the transparent unit that outlet is located at the below and vertically installs, the material of described Gas-phase reactor is recommended as colourless transparent glass or quartzy material, described Gas-phase reactor periphery is provided with the telescopic darkening ring of may command illumination optical throughput (5), described chloridating gas feeds the top that mouth is located at Gas-phase reactor, described condenser one end and Gas-phase reactor outlet are joined, the condenser the other end connects gas-liquid separator, described gas-liquid separator output terminal is the pneumatic outlet that makes progress of opening and the liquid exit that Open Side Down, described liquid exit communicates with the rectifying column bottom by the phegma tube sealing, described phegma tube sealing is a U-shaped pipe, described U-shaped pipe is connected an end with gas-liquid separator (7) level attitude is higher than the other end that communicates with the rectifying column bottom, an end that is connected with the rectifying column bottom is the level of state described reactor, rectifying column, adjustable pipe, folding shape pipe, Gas-phase reactor, condenser, gas-liquid separator, the phegma tube sealing, rectifying column bottom sealing successively is communicated with the circulation line that constitutes reaction system.Described reactor can be prepared different sizes according to reaction needed.
The device of embodiment 2 usefulness embodiment 1 prepares high-content one chloropinacolone
Install the device of embodiment 1 on the 500L glassed steel reaction vessels, nitrogen tube and chlorine tube and inlet pipe are joined, inlet pipe is connected on the chloridating gas ingress, and the pneumatic outlet of gas-liquid separator connects the hydrogen chloride absorption device, the total system nitrogen replacement; The 352Kg pinacolone is added reactor, inject a little above-mentioned raw materials blocking-up gas in the phegma tube sealing and pass through, reactor begins heating, after the raw material boiling, raw material vapor enters Gas-phase reactor through rectifying column, adjustable pipe, folding shape pipe, enters gas-liquid separator after continuing to flow to condenser; Light source is a natural light, after flow of feed gas is stable, when the Gas-phase reactor temperature in reaches 105 ℃, open chloridating gas inlet pipe valve, this moment, reaction was carried out at once, carry out optical chlorinating reaction in the reactor from top to down, the chloropinacolone, hydrogenchloride and the unreacted pinacolone that generate, immediately along air flow line downwards through condenser condenses, raw material, a chloropinacolone are separated with the hydrogenchloride of generation through gas-liquid separator, hydrogenchloride removes absorption unit, and raw material, a chloropinacolone flow into reactor through the phegma tube sealing; Control rate of heating and chloridating gas feeding amount keep stable and reflux; Along with reaction continue carry out, reactor temperature can continue to rise, and when waiting to reach 130 ℃, stops logical chlorine, sampling is carried out GC and is analyzed, and the results are shown in Table 1 embodiment 2.
Atmospheric evaporation reclaims unreacting material and applies mechanically, and without rectifying, still liquid is analyzed through GC, and a chloropinacolone content reaches 99.6%. and the method for bibliographical information, needs rectifying just can obtain the product of 97% above content, produces more the more chloro by product waste liquid simultaneously.
The device of embodiment 3 usefulness embodiment 1 prepares high-content one chloropinacolone
With the operating process of device and the embodiment 2 of embodiment 1, tunger tube and chlorine tube and inlet pipe are joined, light source is a ultraviolet light, and chloridating gas is a chlorine, and the Gas-phase reactor temperature in begins logical chlorine when reaching 104 ℃; When reaching 160 ℃ in the question response still, stop logical chlorine, the GC analysis is carried out in sampling, the results are shown in Table 1 embodiment 3.
Atmospheric evaporation reclaims unreacting material and applies mechanically, and without rectifying, still liquid is analyzed through GC, and a chloropinacolone content reaches 99.5%. and the method for bibliographical information, needs rectifying just can obtain the product of 97% above content, produces more the more chloro by product waste liquid simultaneously.
The device of embodiment 4 usefulness embodiment 1 prepares high-content one chloropinacolone
With the operating process of device and the embodiment 2 of embodiment 1, helium tube and chlorine tube and inlet pipe are joined, light source is a daylight light, and chloridating gas is a chlorine, and the Gas-phase reactor temperature in begins logical chlorine when reaching 105 ℃; When reaching 145 ℃ in the question response still, stop logical chlorine, the GC analysis is carried out in sampling, the results are shown in Table 1 embodiment 4.
Atmospheric evaporation reclaims unreacting material and applies mechanically, and without rectifying, still liquid is analyzed through GC, and a chloropinacolone content reaches 99.6%. and the method for bibliographical information, needs rectifying just can obtain the product of 97% above content, produces more the more chloro by product waste liquid simultaneously.
Claims (10)
1. the preparation method of a chloropinacolone, described method is to be raw material with the pinacolone in chlorination reaction device, under light source irradiation, make a corresponding chloropinacolone with chloridating gas generation chlorination reaction, described chlorination reaction device comprises the reactor that has heating unit, be located at the rectifying column of reactor outlet top, be provided with the Gas-phase reactor that chloridating gas feeds mouth, condenser, it is characterized in that: described chlorination reaction device also comprises gas-liquid separator and phegma tube sealing, rectifying column is suitable for reading to be connected with Gas-phase reactor by folding shape pipeline, described Gas-phase reactor is located at the top for inlet, outlet is located at below and vertically arranged transparent unit, described Gas-phase reactor periphery is provided with illumination apparatus, described chloridating gas feeds the top that mouth is located at Gas-phase reactor, air flow line is vertically downward in the described Gas-phase reactor when guaranteeing chlorination reaction, described condenser one end and Gas-phase reactor outlet are joined, the other end connects gas-liquid separator, described gas-liquid separator output terminal comprises pneumatic outlet and liquid exit, described liquid exit communicates described reactor by the phegma tube sealing with rectifying column bottom or reactor upper interface, rectifying column, the pipeline of folding shape, Gas-phase reactor, condenser, gas-liquid separator and phegma tube sealing, rectifying column bottom or reactor upper interface are communicated with the circulation line that constitutes reaction system successively.
2. the preparation method of a chloropinacolone as claimed in claim 1 is characterized in that, described raw material is a pinacolone, makes a corresponding chloropinacolone with chloridating gas generation chlorination reaction under light source irradiation.
3. the preparation method of a chloropinacolone according to claim 1, described method: dropping into described pinacolone in reactor is raw material, and stay a little raw material and in the phegma tube sealing, inject, reach the fluid-tight effect, open the heating unit of reactor, reflux, the temperature in for the treatment of Gas-phase reactor reaches and is lower than 2 ℃ of raw material boiling temperatures, and when the condenser outlet at bottom has backflow, slowly open the chloridating gas intake valve, under the illumination apparatus irradiation, the pinacolone raw material and the chloridating gas generation chlorination reaction that are generated by the reactor heating and gasifying generate a chloropinacolone, by condenser condenses air inlet liquid/gas separator are arranged simultaneously, and it is acid that tail gas is, control reactor rate of heating and chloridating gas feeding amount keep stable and reflux; Along with the reaction continue carry out, reactor temperature can continue to rise, the question response temperature in the kettle reaches when hanging down in 10 ℃～50 ℃ scopes than a chloropinacolone boiling point, stop logical chloridating gas, product evaporates under normal pressure removes raw material, residuum is mainly a chloropinacolone, and described chloridating gas is the mixed gas of the arbitrary proportion of chlorine or chlorine and rare gas element, and described rare gas element is nitrogen, helium or argon gas.
4. one kind is used for the isolated plant of chloromethyl compound preparation according to claim 1, described isolated plant comprises the reactor that has heating unit, be located at the rectifying column of reactor outlet top, be provided with the Gas-phase reactor that chloridating gas feeds mouth, condenser, it is characterized in that, described chlorination reaction device also comprises gas-liquid separator and phegma tube sealing, described rectifying column is connected with Gas-phase reactor by folding shape pipeline, described Gas-phase reactor is located at the top for inlet, outlet is located at below and vertically arranged transparent unit, described Gas-phase reactor periphery is provided with light source light according to device, described chloridating gas feeds the top that mouth is located at Gas-phase reactor, described condenser one end and Gas-phase reactor outlet are joined, the other end connects gas-liquid separator, described gas-liquid separator output terminal comprises pneumatic outlet and liquid exit, described liquid exit communicates described reactor by the phegma tube sealing with rectifying column bottom or reactor upper interface, rectifying column, the pipeline of folding shape, Gas-phase reactor, condenser, gas-liquid separator, the phegma tube sealing, rectifying column bottom or reactor upper interface are communicated with the circulation line that constitutes reaction system successively.
5. isolated plant as claimed in claim 4 is characterized in that the outside surface of described Gas-phase reactor is provided with the optical throughput setter of may command intensity of illumination.
6. isolated plant as claimed in claim 5 is characterized in that described optical throughput setter is telescopic darkening ring.
7. isolated plant as claimed in claim 4 is characterized in that described folding shape pipeline is " n " font, and described folding shape pipeline is connected with rectifying column by corrugated tube.
8. isolated plant as claimed in claim 4 is characterized in that described phegma tube sealing is a U-shaped pipe, and described U-shaped pipe is connected an end with prolong level attitude is higher than the other end that is connected with rectifying column bottom or reactor upper interface.
9. isolated plant as claimed in claim 4 is characterized in that described gas-liquid separator pneumatic outlet is connected with the hydrogen chloride absorption device.
10. isolated plant as claimed in claim 4, it is characterized in that described isolated plant comprises the reactor that has heating unit, be located at reactor and export the rectifying column that the top has thermal insulation layer, be provided with the Gas-phase reactor that chloridating gas feeds mouth, condenser, gas-liquid separator and phegma tube sealing, described rectifying column is by adjustable pipe and " n " font folding shape pipe connection, described folding shape pipeline can be installed the chloridating gas inlet pipe, described Gas-phase reactor is located at the top for inlet, outlet is located at below and vertically arranged transparent unit, described Gas-phase reactor periphery is provided with illumination apparatus, chloridating gas feeds the top that mouth is located at Gas-phase reactor, described condenser one end and Gas-phase reactor outlet are joined, the condenser the other end connects gas-liquid separator, described gas-liquid separator output terminal is the pneumatic outlet that makes progress of opening and the liquid exit that Open Side Down, described liquid exit is connected with rectifying column bottom or reactor upper interface by the phegma tube sealing, described phegma tube sealing is a U-shaped pipe, described U-shaped pipe is connected an end with condenser level attitude is higher than the other end that is connected with the rectifying column bottom, described reactor, rectifying column, adjustable pipe, folding shape pipe, Gas-phase reactor, condenser, gas-liquid separator, phegma tube sealing and rectifying column are communicated with the circulation line that constitutes reaction system successively.
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| CN109382060A (en) * | 2018-11-30 | 2019-02-26 | 黄冈师范学院 | Automatically control the method and device that nitric acid nitrating oxidation generates nitrogen oxide speed |
| CN109985589A (en) * | 2017-12-29 | 2019-07-09 | 黄国柱 | Irradiation reacts chemical industry processing system |
| CN114409516A (en) * | 2021-12-02 | 2022-04-29 | 江苏剑牌农化股份有限公司 | Method for preparing high-purity chloropinacolone by photocatalysis |
-
2010
- 2010-02-01 CN CN201010117454A patent/CN101781181A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102247789A (en) * | 2011-06-24 | 2011-11-23 | 威海新元化工有限公司 | Device and method for synthesizing 2-chloro-3,3,3-trifluoropropene |
| CN102247789B (en) * | 2011-06-24 | 2016-02-03 | 威海新元化工有限公司 | A kind of synthesizer of 2-chloro-3,3,3 ,-trifluoropropene and method |
| CN109985589A (en) * | 2017-12-29 | 2019-07-09 | 黄国柱 | Irradiation reacts chemical industry processing system |
| CN109382060A (en) * | 2018-11-30 | 2019-02-26 | 黄冈师范学院 | Automatically control the method and device that nitric acid nitrating oxidation generates nitrogen oxide speed |
| CN109382060B (en) * | 2018-11-30 | 2023-08-22 | 黄冈师范学院 | Method and device for automatically controlling nitric acid nitrification and oxidation to generate nitrogen oxide |
| CN114409516A (en) * | 2021-12-02 | 2022-04-29 | 江苏剑牌农化股份有限公司 | Method for preparing high-purity chloropinacolone by photocatalysis |
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