CN202113843U - Device for preparing chloromethane and ammonia - Google Patents
Device for preparing chloromethane and ammonia Download PDFInfo
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- CN202113843U CN202113843U CN2011202116926U CN201120211692U CN202113843U CN 202113843 U CN202113843 U CN 202113843U CN 2011202116926 U CN2011202116926 U CN 2011202116926U CN 201120211692 U CN201120211692 U CN 201120211692U CN 202113843 U CN202113843 U CN 202113843U
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- dividing plate
- conversion zone
- vertical dividing
- ammonia
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Abstract
The utility model belongs to the technical field of chemical equipment, and relates to a device for preparing chloromethane and ammonia, which comprises a gas-solid separating chamber, a reaction section and an air chamber in sequential connection from top to bottom. Two mutually perpendicular vertical partition plates are arranged in the device, so that a bed is divided into four internally communicated areas, and heat supply, synthetic reaction of the chloromethane, circulation of catalysts and regeneration of carbon deposit catalysts are simultaneously completed in the four areas. By the aid of the device, the problems of transfer of a large amount of heat needed by reaction and equipment material quality can be solved, backmixing of the chloromethane and the ammonia is limited in the axial height of the device, and excellent effects for restraining side reaction are achieved. The device has the advantages of high equipment integration, simple process, high conversion rate, fine selectivity, easiness in control and the like.
Description
Technical field
The utility model belongs to technical field of chemical, is specifically related to a kind of device for preparing chloromethanes and ammonia with ammonium chloride and methyl alcohol gas solid method.
Background technology
In recent years, because China joins alkali industry fast development, produced a large amount of byproduct ammonium chloride.Ammonium chloride is mainly used in production composite fertilizer, but has chlorion problem such as enrichment in soil when using, and consumption reduces just gradually.Therefore, should explore the new application of ammonium chloride actively.When ammonium chloride decomposes, can generate hydrogen chloride and ammonia, but the two separates very difficulty.Generate chloromethanes through introducing methyl alcohol and hcl reaction, simultaneously recyclable ammonia.Chloromethanes is the important source material of synthesizing methyl-chloro-silane, cellulose esters, quaternized thing, herbicide etc., is widely used in aspects such as agricultural chemicals, synthetic rubber, resin, industrial auxiliary agent.Ammonia is to join alkali to produce one of essential raw material, reuse capable of circulation.Thereby ammonium chloride and methyl alcohol prepared in reaction chloromethanes technology not only can solve the problem of dissolving that joins alkali process side product sodium chloride, also can realize the closed cycle of ammonia, play an important role to promoting China to join the alkali industrial expansion.
At twentieth century beginning of the fifties; Olin Mathieson chemical company proposed with the method for ammonium chloride and methyl alcohol prepared in reaction chloromethanes and ammonia (US2755311, US2755316, US3315441); And two types of reaction process are provided: the one, gaseous state ammonium chloride and gaseous state alcohol fed in the fixed bed that catalyst is housed together react; Catalyst is a particulate alumina, and product also has a small amount of methylamine and ether except that chloromethanes, and discovery is added back to accessory substance to react in the raw material again and can be converted into chloromethanes; Another is the catalyst mix with solid ammonium chloride and molten condition, with the alcohol reaction, tells catalyst recycle after the reaction then, and catalyst is a stannous chloride.The solid ammonium chloride gasification is needed more energy, decompose every mole of ammonium chloride of gasification at 350 ℃ and need use the 165.8kJ heat, because the conductivity of heat of ammonium chloride own is poor; Its surface compressed when chance is hot; Inner caking stops further and decomposes, and direct gasification acquires a certain degree of difficulty, and the ammonium chloride gasification result is better when using the high temperature organic solvent instead and making medium; But gaseous state ammonium chloride has very strong corrosivity, requires very high to equipment material.
Twentieth century eighties; Mitsubishi gas chemical company is in its disclosed patent JP57130930, JP58146519 and JP58194823; Reaction process to ammonium chloride and methyl alcohol prepared in reaction chloromethanes and ammonia improves; And further studied selection of catalysts property and product separation method, this technology has been advanced major step to industrialization.Catalyst can be active A l
2O
3, can be active carbon or activated carbon supported alkali metal compound etc. also, the yield of chloromethanes is up to 74%.
In the above-mentioned disclosed patent, adopt fixed bed or fluidized-bed reactor, and must earlier the ammonium chloride decomposition be got in the reactor again.Although the chloromethanes yield of part embodiment can reach than higher level; But owing to carrying out decomposition and synthesizing in two conversion zones of chloromethanes of ammonium chloride; If the hydrogen chloride that ammonium chloride decompose to produce can not with methyl alcohol reaction and consuming rapidly, might be in course of conveying since the fluctuation of temperature once more with the synthesizing chlorinated ammonium of ammonification and blocking pipe.2009; Hebei University of Science and Technology has proposed to adopt the fluidized-bed reactor with the section of promoting and conversion zone to accomplish the reaction of ammonium chloride and methyl alcohol in its disclosed patent CN101579611 and CN101574657; And the Preparation of catalysts method is provided; But the energy consumption of whole process is higher, and hydrogen chloride is also relatively more serious to the corrosion on Equipment problem.
Summary of the invention
The utility model is to overcome the problem that exists in the prior art; A kind of device that utilizes ammonium chloride and methyl alcohol to prepare chloromethanes and ammonia is provided; It can carry out recombination reaction simultaneously in the utility model device; And solved the utility model device simultaneously and given heat and catalyst regeneration problem, had that technological process is short, conversion ratio is high, selectivity is good, energy consumption is low, smooth operation and the characteristics controlled easily.
The utility model adopts following technical scheme to be achieved.
A kind of device for preparing chloromethanes and ammonia of the utility model, it comprises gas solid separation chamber, conversion zone, the air compartment that links to each other successively from top to bottom; One side on top, said gas solid separation chamber is provided with catalyst inlet; The inside of said gas solid separation chamber is provided with two cyclone separators; Wherein the top of first cyclone separator is provided with flue gas outlet; The top of second cyclone separator is provided with the reaction mixture gas outlet, and is positioned at the top of gas solid separation chamber.
The below is provided with gas distributor in the said conversion zone; Above gas distributor, be provided with vertical dividing plate of the length that is cross-shaped and short vertical dividing plate; The vertical dividing plate of said length is from the top of the through gas solid separation chamber of gas distributor, and the vertical dividing plate of said weak point arrives the position, middle and upper part of conversion zone from gas distributor; The two ends, bottom of the vertical dividing plate of said length have first duct and second duct; Outside one side of said conversion zone is provided with ammonium chloride inlet, above the bottom of opposite side, gas distributor, is provided with catalyst outlet, and said ammonium chloride inlet is positioned at the middle part of conversion zone; Import links to each other with flue gas with the methyl alcohol import respectively in the lower end of said air compartment, and said methanol inlet is positioned at the lower end of air compartment, and said gas distributor is positioned at the top of air compartment.
The vertical dividing plate of said length will install inside with short vertical dividing plate and be separated into A, B, C, four zones of D, and be provided with the duct in the bottom of growing vertical dividing plate between the regional A, D and between the area B, C, i.e. first duct and second duct.
Said conversion zone and gas-solid separation chamber are cylinder, and the cross section side ratio of said gas solid separation chamber and conversion zone is 2: 1, and the height of said conversion zone and cross section side ratio are 16: 1～25: 1.The percent opening of said gas distributor is 5%～40%.
The utility model compared with prior art has following significant advantage:
1. in a reactor, realize the reaction of ammonium chloride and methyl alcohol and two processes of catalyst regeneration simultaneously, equipment is simple, technological process is short, small investment.
2. in reaction, solved the catalyst carbon deposit problem.
3. utilize flue gas that reaction institute's calorific requirement and catalyst regeneration institute calorific requirement are provided, greatly reduce energy consumption.
Description of drawings
Fig. 1 prepares the structural representation of the device of chloromethanes and ammonia for the utility model.
Fig. 2 prepares the vertical view of the device of chloromethanes and ammonia for the utility model.
Each part description among the figure:
1 catalyst inlet; 2. gas solid separation chamber; 3. grow vertical dividing plate; 4. conversion zone; 5. lack vertical dividing plate; 6. ammonium chloride enters the mouth; 7. gas distributor; 8. first duct; 9. air compartment; 10. catalyst outlet; 11. methyl alcohol import; 12. flue gas import; 13. reaction mixture gas outlet; 14. flue gas outlet; 15. first cyclone separator; 16. second duct; 17. second cyclone separator.
The specific embodiment
Below in conjunction with accompanying drawing the utility model is done further to specify:
Referring to Fig. 1, Fig. 2, a kind of device for preparing chloromethanes and ammonia of the utility model, it comprises gas solid separation chamber 2, conversion zone 4, the air compartment 9 that links to each other successively from top to bottom; One side on 2 tops, said gas solid separation chamber is provided with catalyst inlet 1; The inside of said gas solid separation chamber 2 is provided with two cyclone separators; Wherein the top of first cyclone separator 15 is provided with flue gas outlet 14; The top of second cyclone separator 17 is provided with reaction mixture gas outlet 13, and is positioned at the top of gas solid separation chamber 2.
The below is provided with gas distributor 7 in the said conversion zone 4; Above gas distributor 7, be provided with vertical dividing plate 3 of the length that is cross-shaped and short vertical dividing plate 5; The vertical dividing plate 3 of said length is from the top of gas distributor through gas solid separation chambers 27, and the vertical dividing plate 5 of said weak point arrives the position, middle and upper part of conversion zone 4 from gas distributor 7; The two ends, bottom of the vertical dividing plate 3 of said length have first duct 8 and second duct 16; Outside one side of said conversion zone 4 is provided with ammonium chloride inlet 6, above the bottom of opposite side, gas distributor 7, is provided with catalyst outlet 10, and said ammonium chloride inlet 6 is positioned at the middle part of conversion zone 4; The lower end of said air compartment 9 links to each other with flue gas import 12 with methyl alcohol import 11 respectively, and said methanol inlet 11 is positioned at the lower end of air compartment 9, and said gas distributor 7 is positioned at the top of air compartment 9.
The vertical dividing plate of said length 3 will install inside with short vertical dividing plate 5 and be separated into A, B, C, four zones of D, and be provided with the duct in the bottom of growing vertical dividing plate 3 between the regional A, D and between the area B, C, i.e. first duct 8 and second duct 16.
Said conversion zone 4 is a cylinder with gas-solid separation chamber 2, and said gas solid separation chamber 2 is 2: 1 with the cross section side ratio of conversion zone 4, and the height of said conversion zone 4 and cross section side ratio are 16: 1～25: 1.
The percent opening of said gas distributor 7 is 5%～40%.
The utility model practical implementation process is:
A. with catalyst A l
2O
3Join the conversion zone 4 through gas solid separation chamber 2 from catalyst inlet 1; By the flue gas of flue gas import 12 to 300～400 ℃ of region D feedings; And to regional A, area B and zone C feeding nitrogen, along with the increase of region D gas speed, the catalyst granules that has heat gets into zone C by region D through short vertical dividing plate 5 tops; Second duct 16 by long vertical dividing plate 3 bottoms one end gets into area B again; Get into regional A via short vertical dividing plate 5 tops then, the last 8 entering region D through first duct of the long vertical dividing plate 3 bottom other ends again realize the circulation of catalyst granules in whole reactor; Because catalyst has heat, in the catalyst granules cyclic process of solid, makes this unit temp be controlled at 320～350 ℃; This temperature is higher than the saturation temperature of methyl alcohol, so that make the methanol steam of entering that condensation not take place, and is ammonium chloride decomposition and the synthetic suitable temperature of chloromethanes.
B. treat the catalyst granules stable circulation, this unit temp be controlled at 320～350 ℃ stable after, feed methanol steam through gas distributor 7 to the area B of conversion zone 4 by methyl alcohol import 11.
C. add raw material ammonium chloride with feeding screw from ammonium chloride inlet 6.
The catalyst granules or the chamber 2 laggard promoting the circulation of qi of undecomposed chloride solid particle entering gas solid separation of d. being carried secretly by gas separate admittedly; Solid particle is because the area B in the conversion zone 4 is returned in the effect of gravity; Catalyst granules of being carried secretly by gas or undecomposed chloride solid particle are after second cyclone separator 17 further separates; Generate chloromethanes and ammonia; And flow out from the top reaction mixture gas outlet 13 of second cyclone separator 17, the material pipe gets into the bottom of conversion zone 4 through the bottom of first cyclone separator 15 for catalyst and unreacted chloride solid particle; Because reaction is at high temperature carried out; Can cause the carbon distribution of catalyst in the course of reaction; The catalyst of the catalyst carbon deposition of carbon distribution gets into regional A by short vertical dividing plate 5 tops, and first duct 8 of one end gets into region D through long vertical dividing plate 3 bottoms again, in the D zone; Flue gas by flue gas import 12 gets into is burnt the carbon distribution on the catalyst granules; Make catalyst regeneration, the catalyst of regeneration gets into zone C by short vertical dividing plate 5 tops, is got into by second duct 16 of the bottom other end of long vertical dividing plate 3 and continues in the area B to use; Decaying catalyst is discharged from the catalyst outlet 10 of conversion zone 4 lower end side.
Claims (4)
1. a device for preparing chloromethanes and ammonia is characterized in that, it comprises gas solid separation chamber (2), conversion zone (4), the air compartment (9) that links to each other successively from top to bottom; One side on top, said gas solid separation chamber (2) is provided with catalyst inlet (1); The inside of said gas solid separation chamber (2) is provided with two cyclone separators; Wherein the top of first cyclone separator (15) is provided with flue gas outlet (14); The top of second cyclone separator (17) is provided with reaction mixture gas outlet (13), and is positioned at the top of gas solid separation chamber (2);
The below is provided with gas distributor (7) in the said conversion zone (4); Be provided with vertical dividing plate of the length that is cross-shaped (3) and short vertical dividing plate (5) in gas distributor (7) top; The vertical dividing plate of said length (3) is from the top of the through gas solid separation chamber (2) of gas distributor (7), and the vertical dividing plate of said weak point (5) arrives the position, middle and upper part of conversion zone (4) from gas distributor (7); The two ends, bottom of the vertical dividing plate of said length (3) have first duct (8) and second duct (16); Outside one side of said conversion zone (4) is provided with ammonium chloride inlet (6), is provided with catalyst outlet (10) in the bottom of opposite side, the top of gas distributor (7), and said ammonium chloride inlet (6) is positioned at the middle part of conversion zone (4); The lower end of said air compartment (9) links to each other with flue gas import (12) with methyl alcohol import (11) respectively, and said methanol inlet (11) is positioned at the lower end of air compartment (9), and said gas distributor (7) is positioned at the top of air compartment (9).
2. the device of preparation chloromethanes as claimed in claim 1 and ammonia; It is characterized in that; Vertical dividing plate of said length (3) and short vertical dividing plate (5) will install inside and be separated into A, B, C, four zones of D; And be provided with the duct, i.e. first duct (8) and second duct (16) in the bottom of long vertical dividing plate (3) between regional A, the D and between the area B, C.
3. the device of preparation chloromethanes as claimed in claim 1 and ammonia; It is characterized in that; Said conversion zone (4) and gas-solid separation chamber (2) are cylinder; Said gas solid separation chamber (2) is 2: 1 with the cross section side ratio of conversion zone (4), and the height of said conversion zone (4) and cross section side ratio are 16: 1～25: 1.
4. the device of preparation chloromethanes as claimed in claim 1 and ammonia is characterized in that, the percent opening of said gas distributor (7) is 5%～40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202116926U CN202113843U (en) | 2011-06-22 | 2011-06-22 | Device for preparing chloromethane and ammonia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011202116926U CN202113843U (en) | 2011-06-22 | 2011-06-22 | Device for preparing chloromethane and ammonia |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202113843U true CN202113843U (en) | 2012-01-18 |
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ID=45454942
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011202116926U Expired - Fee Related CN202113843U (en) | 2011-06-22 | 2011-06-22 | Device for preparing chloromethane and ammonia |
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| Country | Link |
|---|---|
| CN (1) | CN202113843U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859513A (en) * | 2016-05-23 | 2016-08-17 | 河南红东方化工股份有限公司 | Production method for chloromethane |
-
2011
- 2011-06-22 CN CN2011202116926U patent/CN202113843U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105859513A (en) * | 2016-05-23 | 2016-08-17 | 河南红东方化工股份有限公司 | Production method for chloromethane |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120118 Termination date: 20130622 |