CN102580711A - Production method for synthesizing melamine catalyst by urea with gas phase method - Google Patents
Production method for synthesizing melamine catalyst by urea with gas phase method Download PDFInfo
- Publication number
- CN102580711A CN102580711A CN201210022119XA CN201210022119A CN102580711A CN 102580711 A CN102580711 A CN 102580711A CN 201210022119X A CN201210022119X A CN 201210022119XA CN 201210022119 A CN201210022119 A CN 201210022119A CN 102580711 A CN102580711 A CN 102580711A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- concentration
- washing
- add
- melamine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Catalysts (AREA)
Abstract
The invention belongs to a catalyst preparation technology, and particularly discloses a production method for synthesizing a melamine catalyst by using urea as a raw material with a gas phase method. The method comprises the following steps: (1), preparation of original gum, namely performing the reaction on sodium silicate and aluminium sulfate to prepare the original gum, wherein the concentration of the sodium silicate is controlled into the range of 21 percent to 26 percent, the concentration of the aluminium sulfate is controlled into the range of 20 percent to 30 percent and the pH value at the end point of the neutralization reaction of the sodium silicate and the aluminium sulfate is controlled into the range of 5 to 6; (2), washing; (3), mixing and beating; (4), soda boiling and chambering; (5), washing; (6), acid soaking; and (7), calcination. The catalyst produced with the method has high strength and low consumption in a fluidized bed reactor, namely, averagely, 0.1 to 1kg of the catalyst is consumed by each ton of melamine; the catalyst has high activity, namely, averagely, each kilogram of catalyst can bear 150 to 400 grams of urea per hour; the catalyst has strong poison resistance and does not need to be activated in the production process; and the catalyst has good fluidization effect and has no bad phenomena of channeling, bubbling and the like in the fluidized bed reactor.
Description
Technical field
The invention belongs to catalyst preparation technology, be specially the production method of the synthetic melamine catalyst of vapor phase method urea.
Background technology
Melamine [(NH
2)
3C
3N
3] that is melamine, be a kind of broad-spectrum Organic Chemicals.Be mainly used in and make melamine-formaldehyde resin (MF); Can be used for making daily utensil, environment-friendly type decoration thick china, fabric finishing agent etc., also can cooperate and make paper treating agent, can be used as coating crosslinking agent and flame retardant chemical treatment agent etc. in addition with ether.
Early stage melamine production raw material is a dicyandiamide, and after nineteen sixties, it is raw material that the suitability for industrialized production melamine begins with urea, under uniform temperature and certain pressure effect, reacts as follows:
6(NH
2)
2CO?→?C
3H
6N
6?+?6NH
3?+?3CO
2
Above-mentioned synthesis technique is divided into two kinds of high pressure liquid phase on-catalytic synthetic method (abbreviation high-pressure liquid phase method) and low-pressure vapor phase catalysis synthesis process (being called for short the low-pressure vapor phase method) according to the difference of chemical reaction condition.High-pressure liquid phase method adopts tower reactor, reaction pressure 7-15MPa, and reaction temperature 380-450 ℃, molten state urea is converted into melamine under the HTHP effect.The low-pressure vapor phase fado adopts fluidized-bed reactor, reaction pressure 0.05-2.5MPa, and reaction temperature 370-420 ℃, urea gasifies rapidly under the acting in conjunction of high-temperature low-pressure and catalyst and is converted into melamine.Low-pressure vapor phase method technology is compared with high-pressure liquid phase method technology; Have advantages such as flow process is short, equipment is few, corrosive medium is little, reduced investment, construction period weak point; So obtained paying close attention to widely and using; Show as low-pressure vapor phase method technology and develop over surplus in the of nearly ten year comparatively rapidly, approximately accounted for 70% of global melamine total output, and this trend also develops continuing.
Though the low-pressure vapor phase method technology of melamine has obtained extensive use; But receive the supporting of no corresponding special efficient catalyst for a long time; Problems such as the production capacity that makes low-pressure vapor phase method list overlap the melamine device is difficult to be greatly enhanced, and device ubiquity catalyst consumption height, melamine quality instability, raw material material and energy resource consumption advantage are not obvious.
In the melamine low-pressure vapor phase method process units of China, the catalyst that present stage adopts is mainly gross porosity microsphere silica gel, activated alumina microballoon and Alusil microballoon.
The gross porosity microsphere silica gel is as catalyst or catalyst carrier, petrochemical industry is produced, just obtained extensive use from nineteen sixties, but its in the melamine production device as catalyst applications, effect is unsatisfactory.The ubiquity catalytic activity is low, and the urea of silica gel feeds intake to load and generally is lower than 75g/kg.h; Abrasion are high, and melamine per ton need consume 8～15 kilograms in silica gel; Be prone to poison per two weeks even all need activation once weekly, each 4～8 hours consuming time; Fluidized-bed reactor fluidization quality is poor, is embodied in fluid bed and occurs air pocket easily, and the bed vibrations are big.The activated alumina microballoon is as the melamine catalyst, and is high than gross porosity microsphere silica gel catalytic activity, and urea feeds intake to load and can reach 80～130g/kg.h; Wear and tear also lowly than the gross porosity microsphere silica gel, melamine per ton consumes 3～5 kilograms of activated alumina microballoons; Also be difficult for poisoning; Fluid effect is also good than the gross porosity microsphere silica gel; But it exists critical defect to be: the sticking especially easily filter bag of the accessory substance that its catalysis generates makes that the filter bag pressure reduction rising of melamine device is very fast, two weeks of life of bag filter less than.The filter bag consumption is big, and labor strength is big, and the maintenance of equipment environment is poor, and it is hard to carry on finally to cause device to be produced.Through the experiment of a large amount of production practices and lab scale, find that the Alusil microballoon is best suited for the melamine production catalyst, but problem such as common in the market si-al catalyst microspheres also exists intensity undesirable, and catalyst activity is not good enough.
Summary of the invention
The present invention just is being based on above technical problem, provides that a kind of intensity is good, catalytic activity is high, selectivity good; China's low-pressure vapor phase method melamine production device single line production capacity is enough maximized; The production method of the efficient melamine catalyst that the production cycle is long.
Technical scheme of the present invention is:
The production method of the synthetic melamine catalyst of vapor phase method urea comprises following steps:
(1) system virgin rubber: by bubble flower alkali and reacting aluminum sulfate glue, the concentration of bubble flower alkali is controlled at 21%--26%, and the concentration of aluminum sulfate is controlled at 20%--30%, and it is 5-6 that the reaction end of bubble flower alkali and aluminum sulfate neutralization reaction is controlled at pH value;
(2) washing: the stirring of the reaction solution in the step () is stopped postprecipitation, take out upper water, add deionized water again, stir the parked and deposition in back, repeated water washing 4-6 time is to remove the sodium sulphate that produces in the course of reaction;
(3) mix making beating: add aluminium hydroxide and nitric acid mixing making beating behind the washing colloid, beating time is 10-24 hour;
(4) mist projection granulating: the control EAT is 400 ℃-420 ℃, and leaving air temp is 110 ℃-120 ℃;
(5) soda boiling reaming: add the NaOH of 10%--30%, temperature is controlled at 90 ℃-100 ℃, and the soda boiling time is 1-2 hour;
(6) washing: carry out repeated water washing with deionized water, washing times is at least twice, with centrifuge water is removed and dries, and removes sodium metasilicate, sodium aluminate that dereaction generates, the water-solubility impurity of unreacted NaOH;
(7) soak: add phosphoric acid to flooding material, immersion is the acid site for the fortifying catalytic agent, strengthens catalyst activity;
(8) calcining: under 600 ℃-650 ℃, calcine, calcination time is 1-3 hour;
(9) packing: adopt air to carry out hybrid refrigeration, be 0.2-0.5 hour cool time, is packaged as finished product.
The production method of the synthetic melamine catalyst of vapor phase method urea need add aluminium hydroxide when mixing making beating, aluminium hydroxide is Powdered, calculates by mass percentage, and the aluminium hydroxide amount of adding is the 20%-50% of aluminum sulfate amount.
Needing to add concentration behind the adding aluminium hydrate powder in the production method of the synthetic melamine catalyst of vapor phase method urea be 30%, calculates by percentage to the quality, and the amount that adds nitric acid is 15% of an aluminium hydroxide amount, mixes making beating then.
Adopting concentration sodium hydroxide in the soda boiling in the production method of the synthetic melamine catalyst of vapor phase method urea in the step (seven) is 10%-30%.
The acid that soak adopted in the production method of the synthetic melamine catalyst of vapor phase method urea in the step (seven) is phosphoric acid, and concentration of phosphoric acid is 5%--10%, and soak time is 2-5 hour.
Virgin rubber is meant Alusil, to steep the reaction of colored alkali and aluminum sulfate acid-base neutralization.The concentration of bubble flower alkali is controlled at 21%--26%, and the concentration of aluminum sulfate is controlled at 20%--30%.Two kinds of raw material all need be used high-class product, to reduce bringing into of impurity, influence product quality.It is that 5-6 is advisable that reaction end is controlled at pH value.
Hydro-oxidation aluminium powder and nitric acid mixing making beating in the step (three), aluminium hydrate powder plays the double action of filler and bonding agent, and nitric acid is to dissolve aluminium hydrate powder for acid to make it have bond effect.In addition, the silica alumina ratio of the addition scalable catalyst of control aluminium hydrate powder, thereby control activity of such catalysts.
Mist projection granulating is to make the granularity of catalyst be controlled in the suitable scope of fluid bed through operating parameters such as the frequency of control atomizer, EAT, inlet amounies.
The soda boiling reaming is because of the product hole of magma production is many but the hole is thin, is unfavorable for the parsing of catalyst, and this is the main cause that silica gel is poisoned easily.Through adding the NaOH of 10%--30%, temperature is controlled at 90 ℃-100 ℃, and the time is 1-2 hours, but average pore size enlarges 30%-50%.
Washing in the step (six) is in order to remove sodium metasilicate, the sodium aluminate that dereaction generates, impurity such as unreacted NaOH.
The purpose of soaking in the soak is the acid site for the fortifying catalytic agent, strengthens catalyst activity.
Calcining, under 600 ℃-650 ℃, calcining one is for the curing catalysts structure, increases its intensity, the 2nd, in order to change the unreacted crystalline structure of aluminium hydrate powder completely, make it change activated alumina into, increase the catalytic efficiency of product.
Sodium metasilicate (Na
2SiO
3) have another name called and steep flower alkali, waterglass.
The catalyst basic index that the present invention produces is following:
| Chemical property | Unit | Be not less than | Be not more than | Remarks |
| Burning decrement | Weight % | —— | 4 | In calcining more than 800 ℃ |
| Gama-alumina | Weight % | 10 | 30 | ? |
| Sulphur | ppm | —— | 500 | ? |
| Fe 2O 3 | Weight % | —— | 0.15 | ? |
| Chlorine | ppm | —— | 50 | ? |
| Na 2O | Weight % | —— | 0.2 | ? |
| Physical property | ? | |||
| Specific surface | Meters squared per gram | 120 | —— | ? |
| Pore volume | Milliliter/gram | 0.2 | 0.5 | ? |
| Bulk density | Grams per milliliter | 0.8 | 0.95 | ? |
| Abrasion index | Weight % | —— | 4 | ? |
| Granularity (laser mensuration) | ? | |||
| ＞425 microns | Weight % | —— | 2 | ? |
| 125～425 microns | Weight % | 85 | —— | ? |
| < 125 microns | Weight % | —— | 13 | ? |
Compared with prior art, beneficial effect of the present invention is:
(1), the catalyst produced with this method has the intensity height, in fluid bed, consumes low characteristics, on average produces 0.1 to 1 kilogram of melamine spent catalyst per ton;
(2), the product catalytic efficiency is high, average per kilogram per hour can catalyzing urea 150-400 gram.
(3), mithridatism is strong, need not activation in the production process.
(4), fluid effect is good, and bad phenomenon such as channel, air pocket do not take place in fluidized-bed reactor.
Description of drawings:
Fig. 1 is technological process of production figure of the present invention.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is made further detailed description.
But should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Embodiment 1:
With the concentration that configures is that 20% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 22% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and control reaction end ph value is 5.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 3kg, 30% nitric acid 0.45kg, deionized water 120L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 400 ℃, and leaving air temp is 110 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 10% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 1 hour.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 5% concentration soaked 2 hours to flooding material 10cm.With the 610 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Embodiment 2:
With the concentration that configures is that 25% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 26% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and control reaction end ph value is 6.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 3kg, 30% nitric acid 0.45kg, deionized water 120L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 410 ℃, and leaving air temp is 120 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 20% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 1 hour.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 10% concentration soaked 2 hours to flooding material 10cm.With the 620 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Embodiment 3:
With the concentration that configures is that 20% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 21% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and the control reaction end is ph5.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 5kg, 30% nitric acid 0.75kg, deionized water 120L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 420 ℃, and leaving air temp is 120 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 10% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 1 hour.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 5% concentration soaked 2 hours to flooding material 10cm.With the 630 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Embodiment 4:
With the concentration that configures is that 20% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 22% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and the control reaction end is ph5-6.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 5kg, 30% nitric acid 0.75kg, deionized water 150L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 420 ℃, and leaving air temp is 120 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 20% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 1.5 hours.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 10% concentration soaked 2 hours to flooding material 10cm.With the 650 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Embodiment 5:
With the concentration that configures is that 30% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 22% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and control reaction end ph value is 5.5.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 5kg, 30% nitric acid 0.75kg, deionized water 150L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 420 ℃, and leaving air temp is 110 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 30% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 2 hours.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 10% concentration soaked 2 hours to flooding material 10cm.With the 640 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Embodiment 6:
With the concentration that configures is that 30% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 26% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and the control reaction end is ph6.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 7.5kg, 30% nitric acid 1.2kg, deionized water 150L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 420 ℃, and leaving air temp is 110 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 10% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 1 hour.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 5% concentration soaked 2 hours to flooding material 10cm.With the 630 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Embodiment 7:
With the concentration that configures is that 30% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 26% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and control reaction end ph value is 5.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 7.5kg, 30% nitric acid 1.2kg, deionized water 150L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 400 ℃, and leaving air temp is 110 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 20% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 1 hour.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 10% concentration soaked 2 hours to flooding material 10cm.With the 650 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Embodiment 8:
With the concentration that configures is that 30% aluminum sulfate 50kg places in the 300L stainless steel cauldron, starts stirring, is that 26% sodium silicate solution adds agitated reactor with the speed of 5L/min with the concentration that configures, and control reaction end ph value is 5.Stop after reaction is reached home stirring, quiescent setting is drained upper water with the vacuum machine.In agitated reactor, add deionized water 150L, start and stirred 20 minutes, quiescent setting is drained upper water with the vacuum machine, and so repeated water washing is 4 times.Add aluminium hydrate powder 7.5kg, 30% nitric acid 1.2kg, deionized water 120L start to stir and mix making beating 24 hours.Add the water deionized water according to the denseness of slurries and regulate, so that centrifugal spray drying.The control EAT is 420 ℃, and leaving air temp is 120 ℃ and carries out spray granulating and drying.The product that drying is come out is reinstalled in the stainless steel cauldron, and the liquid caustic soda that adds 30% concentration starts and stirs and electrical heating to flooding material 20cm, temperature is risen to more than 90 ℃ soda boiling 2 hours.Alkali is emitted,, water is deviate from and in oven dry with centrifuge with deionized water repeated water washing 5 times.To dry the product stainless steel cauldron of packing into, the phosphoric acid that adds 10% concentration soaked 2 hours to flooding material 10cm.With the 650 ℃ of calcinings of stainless steel rotation calcining kiln temperature control 1 hour of packing into after the material taking-up, discharging is packaged into finished product after in air, cooling off screening in 5 hours.
Catalyst effect embodiment: the catalyst in order to top method preparation carries out the effect comparative experiments with silica gel and aluminium oxide catalyst, tests branch intensity and catalytic efficiency two parts and carries out.
Embodiment 9: intensity experiment
10 grams are put into drier after respectively at oven dry in 200 ℃ of baking ovens by the microballoon of above method preparation be cooled to the tubular type air-flow abrasion appearance of packing into behind the normal temperature; With 1500ml/min air-flow velocity boiling 60 minutes, record its abrasion loss and be respectively 1.2%, 1.7%, 1.6%, 1.5%, 1.3%, 1.2%, 1.4%, 1.8%.
Embodiment 11: intensity experiment
The microballoon of 10 gram silica gel, aluminum oxide micro-spheres and this method preparation is put into drier after respectively at oven dry in 200 ℃ of baking ovens be cooled to the tubular type air-flow abrasion appearance of packing into behind the normal temperature; With 1500ml/min air-flow velocity boiling 60 minutes; Record its abrasion loss and be respectively silica gel 6%, aluminium oxide 3.8%, the catalyst microballoon of this method preparation is 1.4%.
Embodiment 12: the catalytic efficiency experiment
Under following operating mode, the catalytic efficiency of catalyst is assessed with the yield of melamine.
Carrier gas: ammonia
Carrier gas flux: 1500ml/min
Reaction temperature: 395 ± 1 ℃
Liquid materials flow amount: 50 gram/h
Loaded catalyst: 250 grams
The result of reaction is 3.62g/h for silica gel melamine yield, and the melamine yield of aluminum oxide micro-sphere is 6.45g/t, and the catalyst melamine yield that uses the embodiment of the invention 1 to 8 to make is 9.67g/t-12.09g/h.
Claims (5)
1. vapor phase method urea synthesizes the production method of melamine catalyst, it is characterized in that comprising following steps:
(1) system virgin rubber: by bubble flower alkali and reacting aluminum sulfate glue, the concentration of bubble flower alkali is controlled at 21%--26%, and the concentration of aluminum sulfate is controlled at 20%--30%, and it is 5-6 that the reaction end of bubble flower alkali and aluminum sulfate neutralization reaction is controlled at pH value;
(2) washing: the stirring of the reaction solution in the step () is stopped postprecipitation, take out upper water, add deionized water again, stir the parked and deposition in back, repeated water washing 4-6 time is to remove the sodium sulphate that produces in the course of reaction;
(3) mix making beating: add aluminium hydroxide and nitric acid mixing making beating behind the washing colloid, beating time is 10-24 hour;
(4) mist projection granulating: the control EAT is 400 ℃-420 ℃, and leaving air temp is 110 ℃-120 ℃;
(5) soda boiling reaming: add the NaOH of 10%--30%, temperature is controlled at 90 ℃-100 ℃, and the soda boiling time is 1-2 hour;
(6) washing: carry out repeated water washing with deionized water, washing times is at least twice, with centrifuge water is removed and dries, and removes sodium metasilicate, sodium aluminate that dereaction generates, the water-solubility impurity of unreacted NaOH;
(7) soak: add phosphoric acid to flooding material, immersion is the acid site for the fortifying catalytic agent, strengthens catalyst activity;
(8) calcining: under 600 ℃-650 ℃, calcine, calcination time is 1-3 hour;
(9) packing: adopt air to carry out hybrid refrigeration, be 0.2-0.5 hour cool time, is packaged as finished product.
2. the production method of the synthetic melamine catalyst of vapor phase method urea according to claim 1; It is characterized in that: when mixing making beating, need add aluminium hydroxide; Aluminium hydroxide is Powdered, calculates by mass percentage, and the aluminium hydroxide amount of adding is the 20%-50% of aluminum sulfate amount.
3. the production method of the synthetic melamine catalyst of vapor phase method urea according to claim 2; It is characterized in that: needing to add concentration behind the adding aluminium hydrate powder be 30%; Calculate by percentage to the quality, the amount that adds nitric acid is 15% of an aluminium hydroxide amount, mixes making beating then.
4. the production method of the synthetic melamine catalyst of vapor phase method urea according to claim 1 is characterized in that: adopting concentration sodium hydroxide in the soda boiling in the described step (seven) is 10%-30%.
5. the production method of the synthetic melamine catalyst of vapor phase method urea according to claim 1, it is characterized in that: the acid that soak adopted in the described step (seven) is phosphoric acid, and concentration of phosphoric acid is 5%--10%, and soak time is 2-5 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210022119 CN102580711B (en) | 2012-02-01 | 2012-02-01 | Production method for synthesizing melamine catalyst by urea with gas phase method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210022119 CN102580711B (en) | 2012-02-01 | 2012-02-01 | Production method for synthesizing melamine catalyst by urea with gas phase method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102580711A true CN102580711A (en) | 2012-07-18 |
| CN102580711B CN102580711B (en) | 2013-11-06 |
Family
ID=46470264
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210022119 Active CN102580711B (en) | 2012-02-01 | 2012-02-01 | Production method for synthesizing melamine catalyst by urea with gas phase method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102580711B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106902799A (en) * | 2017-02-17 | 2017-06-30 | 鲁西催化剂有限公司 | A kind of preparation method for synthesizing aluminum silica gel high |
| CN113694911A (en) * | 2021-09-16 | 2021-11-26 | 四川金象赛瑞化工股份有限公司 | Catalyst for synthesizing melamine and preparation method thereof |
| CN113694912A (en) * | 2021-09-16 | 2021-11-26 | 四川金象赛瑞化工股份有限公司 | Catalyst for melamine production and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1545648A1 (en) * | 1965-12-24 | 1969-08-07 | Bergwerksverband Gmbh | Process and plant for the production of melamine |
| CN1257754A (en) * | 1999-12-23 | 2000-06-28 | 化学工业部天津化工研究设计院 | Process for preparing Si-Al catalyst carrier |
| CN1493565A (en) * | 2003-09-17 | 2004-05-05 | 丁泽华 | Trimeric cyanamide joint production method using one step method |
| CN101024171A (en) * | 2007-03-28 | 2007-08-29 | 德清县三龙催化剂有限公司 | Catalyst for synthesizing melamine and preparing method |
-
2012
- 2012-02-01 CN CN 201210022119 patent/CN102580711B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE1545648A1 (en) * | 1965-12-24 | 1969-08-07 | Bergwerksverband Gmbh | Process and plant for the production of melamine |
| CN1257754A (en) * | 1999-12-23 | 2000-06-28 | 化学工业部天津化工研究设计院 | Process for preparing Si-Al catalyst carrier |
| CN1493565A (en) * | 2003-09-17 | 2004-05-05 | 丁泽华 | Trimeric cyanamide joint production method using one step method |
| CN101024171A (en) * | 2007-03-28 | 2007-08-29 | 德清县三龙催化剂有限公司 | Catalyst for synthesizing melamine and preparing method |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106902799A (en) * | 2017-02-17 | 2017-06-30 | 鲁西催化剂有限公司 | A kind of preparation method for synthesizing aluminum silica gel high |
| CN106902799B (en) * | 2017-02-17 | 2020-03-27 | 鲁西催化剂有限公司 | Preparation method of synthetic high-alumina silica gel |
| CN113694911A (en) * | 2021-09-16 | 2021-11-26 | 四川金象赛瑞化工股份有限公司 | Catalyst for synthesizing melamine and preparation method thereof |
| CN113694912A (en) * | 2021-09-16 | 2021-11-26 | 四川金象赛瑞化工股份有限公司 | Catalyst for melamine production and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102580711B (en) | 2013-11-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102049314B (en) | Microspherical ethylene oxychlorination catalyst preparation method | |
| CN113617353B (en) | Preparation method of silicon carbide-based silver nano catalyst and application of silicon carbide-based silver nano catalyst in ethylene oxide synthesis | |
| CN101205066B (en) | Macroporous microsphere silica gel preparation thereof | |
| CN102580711B (en) | Production method for synthesizing melamine catalyst by urea with gas phase method | |
| CN108339548A (en) | A kind of nickel/aluminium oxide catalyst microballoon and preparation method thereof | |
| CN102951656B (en) | Method for synthesizing even-grained ZSM-5 molecular sieves | |
| CN113234217B (en) | Preparation method of solid base catalyst and application of solid base catalyst in continuous production of polyether polyol | |
| CN103878023B (en) | The preparation method of catalyzer for synthesizing vinyl acetate | |
| CN106946278A (en) | A kind of boehmite and preparation method thereof | |
| CN1332761C (en) | Process for preparing load type silicon phoshporus aluminium molecular sieve | |
| CN108889296A (en) | SCR catalyst slurries and its preparation method and application | |
| CN1168659C (en) | Process for preparing active alumina | |
| CN106902799B (en) | Preparation method of synthetic high-alumina silica gel | |
| CN103230800B (en) | A kind of containing gallium iron-base fischer-tropsch Catalysts and its preparation method | |
| CN102274743B (en) | High intercrystal poriness zeolite coating material on surface of porous silicon carbide carrier and preparation method thereof | |
| CN102049260B (en) | Microsphere ethylene oxychlorination catalyst and preparation method thereof | |
| CN109453802A (en) | Molecular sieve catalyst and preparation method thereof, the application in methanol and Benzyl Side-Chain alkylated reaction | |
| CN107189692B (en) | A kind of absorption of silicon titanium aeroge and photocatalysis interior wall coating and preparation method thereof | |
| CN105771998B (en) | A kind of catalyst and its application method preparing hydroxy pivalin aldehyde | |
| CN106944072A (en) | The preparation method of efficient isothermal coal based synthetic gas methanation catalyst | |
| CN202427451U (en) | Gas phase production device for synthesizing melamine catalyst by using urea | |
| CN103028437B (en) | Peptization al binder and preparation method thereof and catalytic cracking catalyst and preparation method thereof | |
| CN107398261A (en) | A kind of preparation method based on Diatomite-based Porous Ceramics composite catalyst | |
| CN102006934B (en) | Catalyst and process for producing the same | |
| CN103386307A (en) | Preparation method for Ni-Mg/Al2O3 catalyst |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |