CN201632248U - Device for preparing methyl chloride and ammonia - Google Patents
Device for preparing methyl chloride and ammonia Download PDFInfo
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- CN201632248U CN201632248U CN2010201245130U CN201020124513U CN201632248U CN 201632248 U CN201632248 U CN 201632248U CN 2010201245130 U CN2010201245130 U CN 2010201245130U CN 201020124513 U CN201020124513 U CN 201020124513U CN 201632248 U CN201632248 U CN 201632248U
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Abstract
The utility model relates to a device for preparing methyl chloride and ammonia by the reaction of ammonium chloride and methanol, which belongs to the technical field of chemical equipment. The device comprises a gas-solid separation chamber (2), a reaction section (3) and a riser section (4) which are respectively in an unequal-diameter barrel shape and are connected from top to bottom in sequence. In the utility model, the decomposition of the ammonium chloride and the synthesis of the methyl chloride are carried out at the same time in a fluidized bed provided with the riser section and the reaction section. By adopting the device, the backmixing of the product methyl chloride and the ammonia is limited on the axial height of the device, and thereby, the good effect is taken on restraining side reaction. The utility model has the advantages of short process flow, high conversion rate, high selectivity, low energy consumption, less equipment investment, stable operation, easy 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 connection alkali production process, there is a large amount of by-product ammonium chloride to generate.At present, ammonium chloride is mainly as agricultural fertilizer, and supply exceed demand, and the ammonium chloride price is paced up and down at low level always.Exploitation to the ammonium chloride downstream product is the focus that people pay close attention to always.For a long time, the exploitation of ammonium chloride downstream product mainly concentrates in the decomposition of ammonium chloride, and its main purpose is to reclaim ammonia, and a large amount of hydrogen chloride that decomposition produces or the outlet of chlorine will become new problem.Chlorinity 66% in the molecule of ammonium chloride, and ammonium chloride per ton in theory produces 0.68t hydrogen chloride or 0.66t chlorine.So in decomposable process, the chlorine element is converted into product rather than hydrogen chloride or chlorine, be more satisfactory method.By ammonium chloride and organic matter reaction, the chlorine in its molecule is introduced in the organic molecule, make decomposable process only reclaim ammonia, purification, compression be can simplify, hydrogen chloride or chlorine process reclaimed, also can make the corrosion of equipment retarded.
Chloromethanes is mainly used in preparation organosilicon polymer and the raw material of further chlorination for other halogenated hydrocarbons.In recent years, the swift and violent expansion of organosilicon production capacity has proposed new requirement to the production of chloromethanes.If can realize producing chloromethanes and ammonia by the ammonium chloride and the methyl alcohol reaction of connection alkaline process by-product, be not only the promotion that China's soda industry is developed in a healthy way, simultaneously, also can change the present situation that organosilicon manufacturer must build supporting chloromethanes device.
At twentieth century beginning of the fifties, method (the CA736417 with ammonium chloride and methyl alcohol prepared in reaction chloromethanes and ammonia has invented in Olin Mathieson chemical company, CA748127, CA748130), two class reaction process are proposed: 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, shrink on the surface 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 and product separation method, this technology has been advanced major step to industrialization.Catalyst can be active A l
2O
3, also can be active carbon or activated carbon supported alkali metal compound or Zinc compounds etc., 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 entered 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.In addition, the energy consumption of whole process is higher, and hydrogen chloride is also relatively more serious to the etching problem of equipment.
Summary of the invention
The purpose of this utility model be in the present technology problem, provide a kind of and prepare the device of chloromethanes and ammonia with ammonium chloride and methyl alcohol, it has the conversion ratio height, selectivity is good, energy consumption is low, smooth operation and the characteristics of control easily.
The utility model is achieved through the following technical solutions:
A kind of device for preparing chloromethanes and ammonia, it comprises gas solid separation chamber 2, conversion zone 3, the lifting section 4 of the not isometrical cylindrical body that links to each other successively from top to bottom; One side on 2 tops, described gas solid separation chamber is provided with catalyst inlet 1, and cyclone separator 8 is positioned at the inside of gas solid separation chamber 2, and the top of described cyclone separator 8 is provided with reaction mixture gas body outlet 12, and is positioned at the top of gas solid separation chamber 2; Be provided with conversion zone heater 9 in the described conversion zone 3; Described lifting section 4 lower ends one side is provided with ammonium chloride inlet 5, another lower end side is provided with decaying catalyst outlet 11, the described inside that promotes section 4 is provided with gas distributor 7, the outside is provided with and promotes section heater 10, the described lower end that promotes section 4 links to each other with methanol inlet 6, and described ammonium chloride inlet 5 is arranged on the top that promotes section 4 bottoms, gas distributor 7.
Preferably, described device arranged outside catalyst overflow mechanism 13, the two ends of described catalyst overflow mechanism 13 link to each other with the top of conversion zone 3 and the bottom that promotes section 4 respectively.
Preferably, described conversion zone 3 is two sections not isometrical cylindrical shells with promoting section 4, and described conversion zone 3 is 2: 1 with the diameter ratio that promotes section 4, and the ratio of height to diameter of described conversion zone 3 is 15: 1～25: 1, and the ratio of height to diameter of described lifting section 4 is 1: 1～5: 1.
Preferably, the ratio of height to diameter of described conversion zone 3 is 18: 1～24: 1, and the ratio of height to diameter that promotes section 4 is 2: 1～4: 1.
Preferably, described methanol inlet 6 is positioned at the lower end that promotes section 4, and described gas distributor 7 is positioned at the top of methanol inlet 6, and the percent opening of described gas distributor 7 is 5%～30%.
Preferably, the percent opening of described gas distributor 7 is 10%～15%.
The utility model compared with prior art has the following advantages:
1. realize two different courses of reaction in a reactor, equipment is simple, technological process is short, small investment.
2. quiet run and control easily, operating cost is few.
3. operate airtight carrying out, no discharging of waste liquid, environmental pollution is little.
Description of drawings
Fig. 1 prepares the structural representation of the device of chloromethanes and ammonia for the utility model;
Fig. 2 has the preparation chloromethanes of catalyst overflow mechanism and the structural representation of ammonia device for the utility model.
Each part description among the figure:
1. catalyst inlet; 2. gas solid separation chamber; 3. conversion zone; 4. promote section; 5. ammonium chloride enters the mouth; 6. methanol inlet; 7. gas distributor; 8. cyclone separator; 9. conversion zone heater; 10. promote the section heater; 11. decaying catalyst outlet; 12. reaction mixture gas body outlet; 13. catalyst overflow mechanism.
The specific embodiment
Below in conjunction with accompanying drawing the utility model is further described:
Referring to Fig. 1 and Fig. 2, device of the present utility model, a kind of device for preparing chloromethanes and ammonia, it comprises gas solid separation chamber 2, conversion zone 3, the lifting section 4 of the not isometrical cylindrical body that links to each other successively from top to bottom; One side on 2 tops, described gas solid separation chamber is provided with catalyst inlet 1, and cyclone separator 8 is positioned at the inside of gas solid separation chamber 2, and the top of described cyclone separator 8 is provided with reaction mixture gas body outlet 12, and is positioned at the top of gas solid separation chamber 2; Be provided with conversion zone heater 9 in the described conversion zone 3; Described lifting section 4 lower ends one side is provided with ammonium chloride inlet 5, the lower end opposite side is provided with decaying catalyst outlet 11, the described inside that promotes section 4 is provided with gas distributor 7, the outside is provided with and promotes section heater 10, the described lower end that promotes section 4 links to each other with methanol inlet 6, and described ammonium chloride inlet 5 is arranged on the top that promotes section 4 bottoms, gas distributor 7.
Described device arranged outside catalyst overflow mechanism 13, the two ends of described catalyst overflow mechanism 13 link to each other with the top of conversion zone 3 and the bottom that promotes section 4 respectively.
Described conversion zone 3 is two sections not isometrical cylindrical shells with promoting section 4, and described conversion zone 3 is 2: 1 with the diameter ratio that promotes section 4, and the ratio of height to diameter of described conversion zone 3 is 15: 1～25: 1, and the ratio of height to diameter of described lifting section 4 is 1: 1～5: 1.
The ratio of height to diameter of described conversion zone 3 is 18: 1～24: 1, and the ratio of height to diameter that promotes section 4 is 2: 1～4: 1.
Described methanol inlet 6 is positioned at the lower end that promotes section 4, and described gas distributor 7 is positioned at the top of methanol inlet 6, and the percent opening of described gas distributor 7 is 5%～30%.
The percent opening of described gas distributor 7 is preferably 10%～15%.
Be arranged on the catalyst overflow mechanism 13 of reactor outside; it links to each other (as shown in Figure 2) with the bottom of the lifting section 4 of conversion zone 3 tops and ammonium chloride respectively; when the close phase height in the conversion zone (this for fluid bed in term) when equaling or exceeding conversion zone 3 tops, catalyst granules or chloride solid particle enter through catalyst overflow mechanism 13 and promote section 4.
Below in conjunction with accompanying drawing 1 and Fig. 2, the specific embodiment of the present utility model is described:
Open ammonium chloride and promote section heater 10, make lifting section 4 temperature reach 90～100 ℃, this temperature is higher than the saturation temperature of methyl alcohol, so that make the methanol steam that enters that condensation not take place.Meanwhile, open conversion zone heater 9, make conversion zone 3 temperature reach 320～350 ℃, this temperature is the suitable temperature that ammonium chloride decomposes and chloromethanes is synthetic.Behind the temperature stabilization, with catalyst A l
2O
3Join lifting section 4 through gas solid separation chamber 2 from catalyst inlet 1, simultaneously, methanol steam is promoted section 4 from the material benzenemethanol inlet 6 that promotes section 4 bottoms through gas distributor 7 feedings.With the increase of gas speed, catalyst granules will all enter conversion zone 3, the normal running of implement device.
Behind the system stability, add raw material ammonium chloride with feeding screw from ammonium chloride inlet 5, ammonium chloride is 0.8: 1～1: 1 with the ratio of the amount of substance of methyl alcohol; And to make the weight space velocity (this is term in the fluid bed) in the reactor be 0.5～1.5 hour
-1
Catalyst granules of being carried secretly by gas or undecomposed chloride solid particle enter the 2 laggard promoting the circulation of qi of gas solid separation chamber to be separated admittedly, solid particle since the effect of gravity return in the conversion zone 3; Catalyst granules of being carried secretly by gas or undecomposed chloride solid particle are after cyclone separator 8 further separates; the chloromethanes and the ammonia that generate; and flow out from the top reaction mixture gas body outlet 12 of cyclone separator 8; solid expects that through the bottom of cyclone separator 8 pipe enters the bottom of conversion zone 3, and decaying catalyst is discharged from the decaying catalyst outlet 11 that promotes section 4 lower end side.
Close phase excessive height in the reaction unit has increased the overflow mechanism of catalyst granules on the basis of Fig. 1 device, this device can adopt overflow pipe or other structure, sees Fig. 2.This device links to each other with the bottom of the lifting section 4 of conversion zone 3 tops and ammonium chloride respectively, and when the close phase in the conversion zone 3 highly equaled or exceeded the conversion zone top, catalyst granules entered through the catalyst overflow mechanism and promotes sections 4.
Claims (6)
1. a device for preparing chloromethanes and ammonia is characterized in that, it comprises gas solid separation chamber (2), conversion zone (3), the lifting section (4) of the not isometrical cylindrical body that links to each other successively from top to bottom; One side on top, described gas solid separation chamber (2) is provided with catalyst inlet (1), cyclone separator (8) is positioned at the inside of gas solid separation chamber (2), the top of described cyclone separator (8) is provided with reaction mixture gas body outlet (12), and is positioned at the top of gas solid separation chamber (2); Be provided with conversion zone heater (9) in the described conversion zone (3); Described lifting section (4) lower end one side is provided with ammonium chloride inlet (5), another lower end side is provided with decaying catalyst outlet (11), the described inside that promotes section (4) is provided with gas distributor (7), the outside is provided with and promotes section heater (10), the described lower end that promotes section (4) links to each other with methanol inlet (6), and described ammonium chloride inlet (5) is arranged on the top that promotes section (4) bottom, gas distributor (7).
2. the device of preparation chloromethanes as claimed in claim 1 and ammonia, it is characterized in that, described device arranged outside catalyst overflow mechanism (13), the two ends of described catalyst overflow mechanism (13) link to each other with the top of conversion zone (3) and the bottom that promotes section (4) respectively.
3. the device of preparation chloromethanes as claimed in claim 1 and ammonia, it is characterized in that, described conversion zone (3) and lifting section (4) are two sections not isometrical cylindrical shells, described conversion zone (3) is 2: 1 with the diameter ratio that promotes section (4), the ratio of height to diameter of described conversion zone (3) is 15: 1～25: 1, and the described ratio of height to diameter that promotes section (4) is 1: 1～5: 1.
4. the device of preparation chloromethanes as claimed in claim 1 and ammonia is characterized in that, the ratio of height to diameter of described conversion zone (3) is 18: 1～24: 1, and the ratio of height to diameter that promotes section (4) is 2: 1～4: 1.
5. the device of preparation chloromethanes as claimed in claim 1 and ammonia, it is characterized in that, described methanol inlet (6) is positioned at the lower end that promotes section (4), and described gas distributor (7) is positioned at the top of methanol inlet (6), and the percent opening of described gas distributor (7) is 5%～30%.
6. the device of preparation chloromethanes as claimed in claim 1 and ammonia is characterized in that, the percent opening of described gas distributor (7) is 10%～15%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010201245130U CN201632248U (en) | 2010-03-08 | 2010-03-08 | Device for preparing methyl chloride and ammonia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010201245130U CN201632248U (en) | 2010-03-08 | 2010-03-08 | Device for preparing methyl chloride and ammonia |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201632248U true CN201632248U (en) | 2010-11-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010201245130U Expired - Fee Related CN201632248U (en) | 2010-03-08 | 2010-03-08 | Device for preparing methyl chloride and ammonia |
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|---|---|
| CN (1) | CN201632248U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408301A (en) * | 2011-11-30 | 2012-04-11 | 河北科技大学 | Method for preparing methyl chloride and ammonia by using ammonium chloride and methanol |
| CN102580628A (en) * | 2012-03-02 | 2012-07-18 | 青海中航资源有限公司 | Device and method for simultaneously producing chloromethane and ammonia by taking ammonium chloride as raw material |
-
2010
- 2010-03-08 CN CN2010201245130U patent/CN201632248U/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408301A (en) * | 2011-11-30 | 2012-04-11 | 河北科技大学 | Method for preparing methyl chloride and ammonia by using ammonium chloride and methanol |
| CN102408301B (en) * | 2011-11-30 | 2014-07-02 | 河北科技大学 | Method for preparing methyl chloride and ammonia by using ammonium chloride and methanol |
| CN102580628A (en) * | 2012-03-02 | 2012-07-18 | 青海中航资源有限公司 | Device and method for simultaneously producing chloromethane and ammonia by taking ammonium chloride as raw material |
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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: 20101117 Termination date: 20110308 |