CN1247552C - Method for producing cyanuric acid by vibration fluidized bed method - Google Patents
Method for producing cyanuric acid by vibration fluidized bed method Download PDFInfo
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- CN1247552C CN1247552C CN03134879.3A CN03134879A CN1247552C CN 1247552 C CN1247552 C CN 1247552C CN 03134879 A CN03134879 A CN 03134879A CN 1247552 C CN1247552 C CN 1247552C
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- Prior art keywords
- fluidized bed
- urea
- vibrated fluidized
- tricyanic acid
- cyanuric acid
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- 238000000034 method Methods 0.000 title claims abstract description 44
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title abstract description 10
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000004202 carbamide Substances 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 23
- 238000005469 granulation Methods 0.000 claims abstract description 14
- 230000003179 granulation Effects 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 4
- 230000008901 benefit Effects 0.000 abstract description 3
- 238000005096 rolling process Methods 0.000 abstract 2
- 239000007789 gas Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 7
- 238000005243 fluidization Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000010923 batch production Methods 0.000 description 2
- 239000003034 coal gas Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000008447 perception Effects 0.000 description 1
- 229910000498 pewter Inorganic materials 0.000 description 1
- 239000010957 pewter Substances 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for producing cyanuric acid by a vibrating fluidized bed method, which is characterized by comprising the following steps: mixing cyanuric acid powder and urea, carrying out ball rolling granulation, adding the mixture into a vibrating fluidized bed, and carrying out hot air heating reaction to obtain cyanuric acid, wherein the ratio of the cyanuric acid powder to the urea is 1.5-2: 1, the operation time is 10-20 minutes, the operation temperature is 100-200 ℃, and the ball rolling speed is 50-120 r/min; the hot air temperature of the vibrated fluidized bed is 280-360 ℃, the vibration frequency is 10-50 Hz, the amplitude is 1-3 mm, and the air speed is 0.1-0.5 m/s. Compared with the prior art, the invention has the characteristics of high product yield, various heat energy forms, suitability for large-scale industrial production, good economic benefit and the like.
Description
Technical field
The present invention relates to a kind of method of producing tricyanic acid with the vibrated fluidized bed method.
Background technology
At present, the industrial production tricyanic acid all is raw material with urea, through heat, makes the urea cracking, generates tricarbimide, and repolymerization becomes tricyanic acid.Because this temperature of reaction just can be finished between 180-340 ℃, and urea just begins fusion about 110 ℃, and serious wall sticking phenomenon occurs.In order to solve this problem that occurs in the production, various production methods have appearred in the industrial production, mainly can be divided into solid phase method and liquid phase method, these two kinds of methods respectively have relative merits, and industrial all have an employing, and wherein the characteristics of solid phase method are as follows:
Solid phase method is the production method of the urea direct heating being carried out hot polymerization.According to the difference of heating means, can be divided into: 1 stationary kiln method, this method are the traditional methods of producing tricyanic acid, also are the main method of domestic present employing.It places urea on the dish of stainless steel, put into the process furnace direct heating, make urea be converted into thick tricyanic acid, though this method is simple to operate, invest less, knowhow is for many years also arranged at home, but exist the energy consumption height, yield is low, labour intensity is big, dust is many, and distinct disadvantage, particularly this method such as the difficult recovery of by-product ammonia are difficult to carry out large-scale commercial production.Therefore this method belongs to and wants complete method for updating.2 kiln processes, many improving one's methods once appearred in the problem at the stationary kiln method exists, kiln process is exactly an example, it heats urea together with the tricyanic acid powder, utilizes the tricyanic acid powder to prevent that urea melting from gluing wall, urea is constantly rotated in rotary kiln finish hot polymerization process.This method makes production
Serialization, quality product improves, and raw material consumption obviously descends, and labor condition improves, but investment is big, and comprehensive benefit is difficult to adopt not as good as the stationary kiln method aborning.3 half circulation methods, according to the problem that rotary kiln exists, half circulation method changes rotary kiln into disc type, urea and tricyanic acid is put into dish together heat, and changes continuous production into batch production again.This method is greatly improved yield owing to possess rotary kiln and stationary kiln simultaneously, and labour intensity falls between, but this method is a batch production, and industrial scale also is difficult to amplify.4 other methods, except that above-mentioned several method, also has the molten metal heating method, this method is positioned over urea in the metal bath of mobile tin pewter composition, utilizes the temperature heating urea of liquid metal, and realizes the serialization of production by metal flow, tool report foreign country once set up large-scale full scale plant, domestic also once had producer to carry out experiment in the eighties, excessive because of investing, and cost is higher is abandoned.Fluidized bed process, promptly with air directly as heating source, utilize the characteristics direct heating urea of fluidized-bed, for fluidisation problem and the sticking wall that solves urea, usually with urea from new granulation, make the small particle urea that particle diameter is 01-03mm, and externally wrap up one deck tricyanic acid powder, carry out fluidisation then,, never see the industrialization report though this method has many countries to carry out research.The whole bag of tricks all has relative merits, is kiln formula method but really can satisfy the production technique that industrial production requires.But there are shortcomings such as energy consumption height, yield is low, labour intensity is big in it.
Summary of the invention
The objective of the invention is problem, adopt the form of vibrated fluidized bed, improve and conduct heat and mass-transfer efficiency at above-mentioned technology existence.
The vibrated fluidized bed (VFB) that the present invention uses is nearly ten years drying plants of development gradually, is characterized in mechanical vibrator is added on the common fluidized-bed (CFB), has strengthened heat and mass transfer process.It can form uniform fluidized state under very low fluidizing gas velocity, because gas-solid, solid affixed touching have been strengthened in the particulate pulse jitter, reduced the cementing machine meeting, improves heat and mass efficient, is the significant improvement of fluidized drier.VFB is similar to the drying principles of CFB, be in the material of fluidized state and add the transmission that warm air carries out heat and quality, be dried gradually, but being the vibrating motor that is installed in the main frame both sides, the difference of the two provides vibration, the setting angle of motor all can be regulated its eccentric distance, thereby can change the amplitude of vertical direction and the haul speed of horizontal direction easily.Vibrational frequency can be regulated by the variable-frequency motor of configuration as required.
For solving the sticking wall problem of urea, on vibrated fluidized bed, carry out the spin experiment earlier, found through experiments, the principal element that influences spin is the ratio and the temperature controlling condition of tricyanic acid powder and urea.When tricyanic acid powder and urea are heated together, because the particle diameter of tricyanic acid powder is much smaller than urea (d=50～100 μ m), frequency perception to vibration is relatively poor, easily by gas fluidized, because the two fluidisation mechanism difference, be difficult to guarantee that two kinds of materials flow synchronously, after these two kinds of material are added vibrated fluidized bed together, if the tricyanic acid powder is very few, the two is difficult for mixed, through experiment, the ratio of tricyanic acid powder and urea is 3-4, and in vibrated fluidized bed inside, because tricyanic acid pruinescence entrained air is gone out, make the ratio of tricyanic acid powder and urea reduce, in the time of near near discharge port, easily produce bonding.Air quantity is little, and urea is difficult to fluidisation, and air quantity is big, and the drag-out of tricyanic acid powder can be excessive, same influence operation.The hot air temperature height easily produces sticking wall, and the temperature low reaction influences granulation slowly, experimental result is passed through relatively, can find that the urea spin adopts vibrated fluidized bed no doubt feasible, but controlling factor is too many, rule is also complicated, by contrast, it is many to adopt the huge rock spin of dividing wall type heating to be easy to, and is about to the tricyanic acid powder with the urea salver of packing into together, and make disk and horizontal plane inclination certain angle, heat in the bottom surface of disk.When disk rotated, the tricyanic acid powder in the dish was heated together with urea, and finishes spin work.By test, earlier urea and tricyanic acid powder are pressed following condition granulation: tricyanic acid powder: urea=1.5～2: 1, the operating time is 10～20 minutes, and service temperature is 100～200 ℃, and the spin rotating speed is 50～120 rev/mins.Urea and tricyanic acid powder are by after the above-mentioned condition granulation, and pellet strength is moderate, and the tricyanic acid powder accounts for about 20%, and by fluidisation and the reaction fully of adjusting process parameter, reaction conditions is also easy to control in vibrated fluidized bed.Material after the granulation is added in the vibrated fluidized bed, 280～360 ℃ of hot blast temperatures, vibrational frequency 10～50Hz, amplitude 1～3mm, react under the condition of gas speed 0.1～0.5m/s, for guaranteeing the necessary reaction times, adopt the many series connection mode of heating continuously, the hot blast heating can be adopted, liquefied gas, coal gas, wet goods, using liquefied gas, coal gas, when adding warm air, wet goods can directly get its stack gas, because burning consumes part oxygen, make the oxygenolysis side reaction of urea reduce, help improving product yield, be noted that and fully burn, otherwise the carbon monoxide that produces can make the people poison, and needs to increase to remove equipment or sealing equipment accordingly, and increase equipment drops into.And the carbon black that produces will influence the outward appearance and the quality of product.Vibrated fluidized bed can be selected vertical or horizontal vibrated fluidized bed for use according to practical situation.Reacted material is thick tricyanic acid, and process for purification promptly gets the product tricyanic acid after making with extra care routinely.
The present invention compared with prior art has following advantage: product yield height, characteristics such as heat energy is various informative, is fit to large-scale commercial production, and is good in economic efficiency.
Embodiment
Embodiment 1
Tricyanic acid powder and urea are carried out the spin granulation by 1.5: 1 mixed, 150 ℃ of service temperatures, 10 minutes operating times, 80 rev/mins of spin rotating speeds, the spherical material after the granulation directly adds vibrated fluidized bed without cooling, fluidized-bed is for to be in series by four vibrated fluidized beds, at 300～320 ℃ of hot blast temperatures, vibrational frequency 20Hz, amplitude 1mm, react under the condition of gas speed 0.2m/s, hot blast adopts electrically heated.The transformation efficiency of material is 86%.
Embodiment 2
Tricyanic acid powder and urea are carried out the spin granulation by 2: 1 mixed, 200 ℃ of service temperatures, 15 minutes operating times, 120 rev/mins of spin rotating speeds, the spherical material after the granulation directly adds vibrated fluidized bed without cooling, fluidized-bed is for to be in series by four vibrated fluidized beds, at 280～300 ℃ of hot blast temperatures, vibrational frequency 40Hz, amplitude 3mm, react under the condition of gas speed 0.5m/s, hot blast adopts electrically heated.The transformation efficiency of material is 90%.
Embodiment 3
Tricyanic acid powder and urea are carried out the spin granulation by 1.8: 1 mixed, 160 ℃ of service temperatures, 17 minutes operating times, 100 rev/mins of spin rotating speeds, the spherical material after the granulation directly adds vibrated fluidized bed without cooling, fluidized-bed is for to be in series by four vibrated fluidized beds, at 340～360 ℃ of hot blast temperatures, vibrational frequency 10Hz, amplitude 2mm, react under the condition of gas speed 0.4m/s, hot blast is directly introduced from gas fired-boiler stack gas.The transformation efficiency of material is 92%.
Claims (3)
1. a vibrated fluidized bed method is produced the method for tricyanic acid, it is characterized in that: with the tricyanic acid powder mix with urea carry out the spin granulation after, use the hot blast reacting by heating in the adding vibrated fluidized bed; Spin granulation: tricyanic acid powder: urea=1.5～2: 1, the operating time is 10～20 minutes, and service temperature is 100～200 ℃, and the spin rotating speed is 50～120 rev/mins, and disk and horizontal plane are tilted, and heats in the bottom surface of disk; Vibrated fluidized bed reaction: 280～360 ℃ of hot blast temperatures, vibrational frequency 10～50Hz, amplitude 1～3mm, gas speed 0.1～0.5m/s.
2. vibrated fluidized bed method according to claim 1 is produced the tricyanic acid method, and it is characterized in that: vibrated fluidized bed is vertical or horizontal.
3. vibrated fluidized bed method according to claim 1 is produced the tricyanic acid method, it is characterized in that: vibrated fluidized bed is many vibrated fluidized bed series connection.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN03134879.3A CN1247552C (en) | 2003-09-27 | 2003-09-27 | Method for producing cyanuric acid by vibration fluidized bed method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN03134879.3A CN1247552C (en) | 2003-09-27 | 2003-09-27 | Method for producing cyanuric acid by vibration fluidized bed method |
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| Publication Number | Publication Date |
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| CN1600781A CN1600781A (en) | 2005-03-30 |
| CN1247552C true CN1247552C (en) | 2006-03-29 |
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| CN03134879.3A Expired - Fee Related CN1247552C (en) | 2003-09-27 | 2003-09-27 | Method for producing cyanuric acid by vibration fluidized bed method |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102285928B (en) * | 2011-08-29 | 2014-11-26 | 王铁招 | CA (Cyanuric Acid) liquid phase catalytic synthesis method |
| CN108386862A (en) * | 2018-01-13 | 2018-08-10 | 安徽金禾实业股份有限公司 | A kind of heat supply method and device of melamine fluid bed |
| CN115025720B (en) * | 2022-07-04 | 2023-08-22 | 国能(山东)能源环境有限公司 | System and process for preparing cyanuric acid by urea pyrolysis |
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Granted publication date: 20060329 Termination date: 20210927 |