CN105753017A - Urea catalytic hydrolysis method capable of replenishing catalyst on line - Google Patents
Urea catalytic hydrolysis method capable of replenishing catalyst on line Download PDFInfo
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- CN105753017A CN105753017A CN201610056720.9A CN201610056720A CN105753017A CN 105753017 A CN105753017 A CN 105753017A CN 201610056720 A CN201610056720 A CN 201610056720A CN 105753017 A CN105753017 A CN 105753017A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/08—Preparation of ammonia from nitrogenous organic substances
- C01C1/086—Preparation of ammonia from nitrogenous organic substances from urea
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Abstract
The invention discloses a urea catalytic hydrolysis method capable of replenishing catalyst on line. The urea catalytic hydrolysis method is characterized in that any of phosphoric acid, carbonic acid, MgO/eta-Al2O3, a mixture of nickel and iron, titanium dioxide and coal ash is taken as a catalyst; in a urea catalytic hydrolysis process, in order to ensure the amount of the catalyst in a reactor unchanged, the catalyst is dissolved by use of a urea solution in a urea supply box according to the elapse of the catalyst in the urea catalytic hydrolysis reactor so as to obtain a urea-catalyst solution, then, the urea-catalyst solution is added into the hydrolysis reactor, and the losing catalyst in the hydrolysis reactor is timely replenished, so that the defect that a reaction rate is lowered caused by reduction of the catalyst is overcome. The urea catalytic hydrolysis method provided by the invention has the advantages of being relatively high in reaction speed and relatively low in operation cost, and has higher superiority.
Description
Technical field
The present invention relates to a kind of urea seeding hydrolysis method, belong to technical field of chemical material preparation.
Background technology
Existing urea seeding hydrolysis process, all adopts such as Chinese patent literature (CN 101450807A, CN 202490568U) etc.
Be ammonium dihydrogen phosphate and ammonium hydrogen phosphate as catalyst, the acidity of this catalyst is more weak, and Catalysis Rate is slower；It addition,
Catalyst in urea seeding hydrolysis can be drained off a part along with the online blowdown of system in course of reaction, causes catalysis
The loss of agent, the minimizing of catalyst can cause reaction rate to reduce, it is impossible to meets load variations requirement.
Summary of the invention
It is an object of the invention to provide a kind of urea seeding method for hydrolysis adding catalyst online, the catalysis run off can be supplemented in time
Agent, has met the requirement of system loading change, it is ensured that its further reaction speed is accelerated.
To achieve these goals, the present invention is by the following technical solutions:
A kind of urea seeding method for hydrolysis adding catalyst online, comprises the following steps:
1) by deionized water by catalyst dissolution, used catalyst is phosphoric acid, carbonic acid, MgO/ η-Al2O3, nickel and iron mixing
In thing, titanium dioxide and six kinds of flyash any one, wherein phosphoric acid or carbonic acid account for hydrolysis reactor volume 6-12%, MgO/ η-Al2O3、
Nickel and iron mixture, titanium dioxide and flyash loadings concentration are 10-50g/L；
2) urea liquid of 35-55% mass concentration is delivered to hydrolysis reactor from urea storage tank, control hydrolysis of urea reactor
Temperature at 135-180 DEG C, pressure is at 0.4-1.0MPa；Urea-catalyst solution is made to reach the 40-60% of hydrolysis reactor volume；
The urea amount of inserting and the catalyst amount of inserting are calculated as follows:
m1/ w=V × c × ρ1 (1)
m2=V × a × ρ2 (2)
m3=V × 50% × b (3)
In formula: m1For dry urea quality, unit is kg；m2For phosphoric acid or carbonate catalyst quality, unit is kg；m3For MgO/
η-Al2O3, nickel and iron mixture, titanium dioxide or flyash catalyst quality, unit is kg；W is urea solution mass percentage
Content；V is hydrolysis reactor volume, and unit is m3；ρ1For urea solution density, unit is kg/m3；A is that catalyst accounts for
Hydrolysis reactor volumn concentration；ρ2For phosphoric acid or carbonate catalyst density, unit is kg/m3；B is MgO/ η-Al2O3、
Nickel and iron mixture, titanium dioxide or flyash catalyst loading concentration, g/L；C is that urea liquid accounts for hydrolysis reactor volume
Percentage；
3) catalyst is added:
The urea liquid of 35-55% mass concentration is delivered to catalyst tank catalyst-solvent, and the urea liquid volume of conveying is V1,
The volume that catalyst occupies is 2a V1, then needing at catalyst tank injection phosphoric acid or carbonate catalyst quality is m4；MgO/η
-Al2O3, nickel and iron mixture, titanium dioxide or flyash catalyst quality be m5
m4=2a V1ρ2 (4)
m5=2a V1b (5)
Start online blowdown after solution reaction 1-2 week in hydrolysis reactor, open the 6th valve, by hydrolysis reactor
Solution is drained into wastewater disposal basin from bottom, is calculated the concrete volume discharging solution by the first volume flowmeter, and blowdown flow rate scope exists
Between 70-100L, then add same volume from catalyst service tank online by catalyst supply pump and the second volume flowmeter
Urea-catalyst solution.
In technique scheme, described phosphoric acid or carbonic acid are AR；MgO/η-Al2O3, nickel and iron mixture, dioxy
Changing titanium and fly ash grain size distribution is 1～10mm, particle mean size is 4mm；Bulk density about 1200-1300kg/m3；Compare table
Area 1.3 × 105m2/ kg～2.5 × 105m2/kg.Catalyst service tank material is 316L, and outside is provided with heat-insulation layer, operating temperature
For 50-80 DEG C.
The present invention compared with prior art, has the following advantages and the technique effect of high-lighting: the present invention can supplement water the most in time
Solve the catalyst run off in reactor, thus overcome the defect that the reaction rate caused because of the minimizing of catalyst reduces, therefore this
The urea seeding method for hydrolysis that invention provides has the advantage that reaction speed is very fast, operating cost is low relatively.
Accompanying drawing explanation
Fig. 1 is the structural representation of a kind of urea seeding method for hydrolysis embodiment that the present invention provides.
In figure: 1-catalyst service tank；2-agitator；3-catalyst supply pump；4-urea storage tank；5-hydrolysis reactor；6-
Deionized water service tank；7-liquid level gauge on the spot；8-full barrier film liquid level gauge；9-the first volume flowmeter；10-the second volume flowmeter,
12-third volume flowmeter；11-the 7th valve；13-the first valve；14-the second valve；15-the 3rd valve；16-the 4th valve
Door；17-the 5th valve；18-the 6th valve；19-wastewater disposal basin.
Detailed description of the invention
Below in conjunction with the accompanying drawings structure, principle and the course of work of the present invention is further described.
A kind of urea seeding method for hydrolysis adding catalyst online that the present invention provides, it comprises the steps:
1) by deionized water by catalyst dissolution, used catalyst is phosphoric acid, carbonic acid, MgO/ η-Al2O3, nickel and iron mixture,
In titanium dioxide and six kinds of flyash any one, wherein phosphoric acid or carbonic acid account for hydrolysis reactor volume 6-12%, MgO/ η-Al2O3、
Nickel and iron mixture, titanium dioxide and flyash loadings concentration are 10-50g/L；
2) urea liquid of 35-55% mass concentration is delivered to hydrolysis reactor from urea storage tank, control the temperature of hydrolysis of urea reactor
Degree is at 135-180 DEG C, and pressure is at 0.4-1.0MPa；Urea-catalyst solution is made to reach the 40-60% of hydrolysis reactor volume；
The urea amount of inserting and the catalyst amount of inserting are calculated as follows:
m1/ w=V × c × ρ1 (1)
m2=V × a × ρ2 (2)
m3=V × 50% × b (3)
In formula: m1For dry urea quality, unit is kg；m2For phosphoric acid or carbonate catalyst quality, unit is kg；m3For MgO/
η-Al2O3, nickel and iron mixture, titanium dioxide or flyash catalyst quality, unit is kg；W is urea solution mass percentage
Content；V is hydrolysis reactor volume, and unit is m3；ρ1For urea solution density, unit is kg/m3；A is that catalyst accounts for
Hydrolysis reactor volumn concentration；ρ2For phosphoric acid or carbonate catalyst density, unit is kg/m3；B is MgO/ η-Al2O3、
Nickel and iron mixture, titanium dioxide or flyash catalyst loading concentration, g/L；C is that urea liquid accounts for hydrolysis reactor volume
Percentage；
3) catalyst is added:
The urea liquid of 35-55% mass concentration is delivered to catalyst tank catalyst-solvent, and the urea liquid volume of conveying is V1,
The volume that catalyst occupies is 2a V1, then needing at catalyst tank injection phosphoric acid or carbonate catalyst quality is m4；MgO/η
-Al2O3, nickel and iron mixture, titanium dioxide or flyash catalyst quality be m5
m4=2a V1ρ2 (4)
m5=2a V1b (5)
It is embodied as being described further to the present invention below in conjunction with the accompanying drawings:
The structural representation of a kind of embodiment adding urea seeding method for hydrolysis equipment therefor online that Fig. 1 provides for the present invention,
This device contains catalyst service tank 1, urea storage tank 4, hydrolysis reactor 5 and deionized water service tank 6；Described urea storage
Tank 4 is connected with hydrolysis reactor 5 and catalyst service tank 1 by pipeline respectively, at urea storage tank 4 and hydrolysis reactor 5
Connecting line is provided with secondValve14, the connecting line between urea storage tank 4 and catalyst service tank 1 is sequentially provided with
Three valves 15 and third volume flowmeter 12；Described deionized water service tank 6 is respectively by pipeline and valve and hydrolysis
Device 5 and catalyst service tank 1 connect；The bottom of described catalyst service tank 1 is by pipeline and catalyst supply pump 3 and water
Solve reactor 5 to connect, and on pipeline, be provided with the 5th valve 17 and the second volume flowmeter 10；The end at hydrolysis reactor 5
Portion is connected with wastewater disposal basin by pipeline and 19 is connected, and is provided with the 6th valve 18 and the first volume flowmeter 9 on this pipeline.
Start before hydrolysis reactor 5, pour a certain amount of catalyst into catalyst service tank 1, open the 4th valve 16, will go from
Deionized water in sub-water service tank 6 is injected into catalyst service tank 1, and liquid level gauge on the spot 7 and the full barrier film liquid level gauge 8 of configuration are used for
Measuring catalyst tank liquid level, liquid level is higher than 4/5 5/6 warnings of catalyst service tank height, less than catalyst service tank height
1/6 1/5 report to the police, and in the range of liquid level reaches target level, close the 4th valve 16, open agitator 2 catalyst-solvent, dissolve
After completing, open the 5th valve 17 and catalyst supply pump 3, catalyst solution is all injected hydrolysis reactor 5, closes the 5th
Valve 17 and catalyst supply pump 3, open the first valve 13, the deionization in deionized water service tank 6 injected hydrolysis reactor 5,
Make liquid level reach the 25% of hydrolysis reactor 5, close the first valve 13, open the 4th valve 16 simultaneously, use deionized water service tank
In deionized water cleaning catalyst service tank 1, after cleaning, close the 4th valve 16, open the 7th valve 11 and waste water put
Sky, opens the second valve 14 the most simultaneously, and the urea liquid of urea storage tank 4 is injected hydrolysis reactor 5, reaches to solve reactor 5 liquid level
50%, control hydrolysis of urea reactor temperature at 135 180 DEG C, pressure is at 0.4 1.0MPa, it is achieved the catalyzing hydrolysis of urea.
Start online blowdown after solution reaction 1-2 week in hydrolysis reactor, open the 6th valve 18, molten by hydrolysis reactor
Liquid is drained into wastewater disposal basin 19 from bottom, is calculated the concrete volume discharging solution by the first volume flowmeter 9, and blowdown flow rate scope exists
Between 70-100L, then add same volume from catalyst service tank online by catalyst supply pump and the second volume flowmeter
Urea-catalyst solution.
Solution in catalyst service tank is vented from drain 11, by the deionization injecting catalyst in deionized water service tank 6
Service tank 1, is carried out device.
Embodiment
Before starting empty hydrolysis reactor, catalyst is poured catalyst service tank into, by the deionized water in deionized water service tank
Catalyst-solvent, catalyst tank configures full barrier film liquid level gauge and liquid level gauge on the spot, is used for measuring catalyst tank liquid level, catalyst
Case is high 1.8 meters, and liquid level is higher than 1.5 meters of warnings, less than 0.3 meter of warning.Open the agitator 2 at catalyst tank top, be used for
Promote catalyst dissolution, form uniform solution；Catalyst is the amount that phosphoric acid accounts for hydrolysis reactor volume 6%；
Deionization in deionized water service tank 6 is injected hydrolysis reactor 5 and reaches deionization goal-setting liquid level, catalyst is molten
Liquid is squeezed into hydrolysis reactor 5 by high-pressure pump 3, reaches catalyst goal-setting liquid level.Afterwards by the urea liquid of 35% mass concentration from
Urea storage tank delivers to hydrolysis reactor, reaches urea liquid goal-setting liquid level, and all solution account for the 50% of hydrolysis reactor volume；
The temperature of control hydrolysis of urea reactor is at 135 DEG C, and pressure is at 0.4MPa, it is achieved the catalyzing hydrolysis of urea.
According to above-mentioned formula (1)-(3) the calculating urea amount of inserting:
Urea solution mass percentage composition w=35%, its density p1=1.1 × 103kg/m3；Hydrolysis reactor volume V=5.2m3；Urge
Agent accounts for hydrolysis reactor volumn concentration a=6%；Phosphoric acid density p2=1.69×103kg/m3；Dry urea quality m1=1001kg；
Phosphoric acid quality m2=527.3kg.So the dry urea of 1001kg should be added in urea storage tank, being dissolved into weight/mass percentage composition is
The urea liquid of 35%, the most all injects hydrolysis reactor.The catalyst that should add 527.3kg in catalyst service tank spends
Ionized water all injects hydrolysis reactor after dissolving.
According to above-mentioned formula (4)-(5) calculating catalyst additional amount:
1) urea liquid of 35% mass concentration being delivered to catalyst tank catalyst-solvent, urea liquid volume is V1=0.5m3, urge
The volume that agent is occupied is 2a V1=2 × 6% × 0.5=0.06m3；Catalyst quality is m4=0.06 × 1.69 × 103=101.4kg.
Need to pour the phosphoric acid of 101.4kg into catalyst service tank 0.5m335% urea liquid dissolve.
2) utilizing the volume flowmeter on hydrolysis reactor blow-off line to calculate the blowdown flow rate volume discharged is V2, then need from catalysis
Agent case injects same volume V2Urea-catalyst solution.
3) solution in catalyst service tank is vented from drain 11, the deionization in deionized water service tank 6 is injected and urges
Agent service tank 1, is carried out device.
Claims (3)
1. adding a urea seeding method for hydrolysis for catalyst online, the method comprises the following steps:
1) by deionized water by catalyst dissolution, used catalyst is phosphoric acid, carbonic acid, MgO/ η-Al2O3, nickel and iron mixing
In thing, titanium dioxide and six kinds of flyash any one, wherein phosphoric acid or carbonic acid account for hydrolysis reactor volume 6-12%, MgO/ η-Al2O3、
Nickel and iron mixture, titanium dioxide and flyash loadings concentration are 10-50g/L；
2) urea liquid of 35-55% mass concentration is delivered to hydrolysis reactor from urea storage tank, control hydrolysis of urea reactor
Temperature at 135-180 DEG C, pressure is at 0.4-1.0MPa；Urea-catalyst solution is made to reach the 40-60% of hydrolysis reactor volume；
The urea amount of inserting and the catalyst amount of inserting are calculated as follows:
m1/ w=V × c × ρ1 (1)
m2=V × a × ρ2 (2)
m3=V × 50% × b (3)
In formula: m1For dry urea quality, unit is kg；m2For phosphoric acid or carbonate catalyst quality, unit is kg；m3For MgO/
η-Al2O3, nickel and iron mixture, titanium dioxide or flyash catalyst quality, unit is kg；W is urea solution mass percentage
Content；V is hydrolysis reactor volume, and unit is m3；ρ1For urea solution density, unit is kg/m3；A is that catalyst accounts for
Hydrolysis reactor volumn concentration；ρ2For phosphoric acid or carbonate catalyst density, unit is kg/m3；B is MgO/ η-Al2O3、
Nickel and iron mixture, titanium dioxide or flyash catalyst loading concentration, g/L；C is that urea liquid accounts for hydrolysis reactor volume
Percentage；
3) catalyst is added:
The urea liquid of 35-55% mass concentration is delivered to catalyst tank catalyst-solvent, and the urea liquid volume of conveying is V1, urge
The volume that agent is occupied is 2a V1, then needing at catalyst tank injection phosphoric acid or carbonate catalyst quality is m4；MgO/η-Al2O3、
Nickel and iron mixture, titanium dioxide or flyash catalyst quality are m5
m4=2a V1ρ2 (4)
m5=2a V1b (5)
Start online blowdown after solution reaction 1-2 week in hydrolysis reactor, open the 6th valve (18), by hydrolysis
Solution in device is drained into wastewater disposal basin (19) from bottom, is calculated the concrete volume discharging solution by the first volume flowmeter (9)
Amount, blowdown flow rate scope is between 70-100L, then from catalyst service tank (1) by catalyst supply pump (3) and second
Volume flowmeter (10) adds the urea-catalyst solution of same volume online.
A kind of urea seeding method for hydrolysis adding catalyst the most according to claim 1, it is characterised in that: phosphoric acid and
Carbonic acid is AR；MgO/η-Al2O3, nickel and iron mixture, titanium dioxide and fly ash grain size distribution be 1～
10mm, particle mean size is 4mm；Bulk density about 1200-1300kg/m3；Specific surface area 1.3 × 105m2/ kg～2.5 × 105m2/kg。
A kind of urea seeding method for hydrolysis adding catalyst the most according to claim 1, it is characterised in that: catalyst
Service tank material is 316L, and outside is provided with heat-insulation layer, and operating temperature is 50 80 DEG C.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112619637A (en) * | 2020-12-29 | 2021-04-09 | 中国华电科工集团有限公司 | Preparation method of heterogeneous solid catalyst for preparing ammonia by urea hydrolysis |
| CN112661172A (en) * | 2020-12-23 | 2021-04-16 | 中国华电科工集团有限公司 | System and method for preparing ammonia through SCR (selective catalytic reduction) denitration urea heterogeneous catalytic hydrolysis |
| CN113070054A (en) * | 2021-03-02 | 2021-07-06 | 中国华电科工集团有限公司 | Preparation method of non-supported catalyst, product and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661172A (en) * | 2020-12-23 | 2021-04-16 | 中国华电科工集团有限公司 | System and method for preparing ammonia through SCR (selective catalytic reduction) denitration urea heterogeneous catalytic hydrolysis |
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| CN113070054A (en) * | 2021-03-02 | 2021-07-06 | 中国华电科工集团有限公司 | Preparation method of non-supported catalyst, product and application |
| CN113070054B (en) * | 2021-03-02 | 2023-07-14 | 中国华电科工集团有限公司 | Preparation method, product and application of non-supported catalyst |
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Application publication date: 20160713 |