CN112755930A - Production equipment and production process of sulfamic acid - Google Patents
Production equipment and production process of sulfamic acid Download PDFInfo
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- CN112755930A CN112755930A CN202011601654.1A CN202011601654A CN112755930A CN 112755930 A CN112755930 A CN 112755930A CN 202011601654 A CN202011601654 A CN 202011601654A CN 112755930 A CN112755930 A CN 112755930A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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Abstract
The application relates to the field of sulfamic acid preparation, and particularly discloses equipment and a process for producing sulfamic acid. The utility model provides a sulfamic acid production facility uses the hair-dryer pay-off of blowing to carry out the breakage to urea, uses with the cooperation of temperature allies oneself with accuse subassembly simultaneously for urea intermittent type nature is reinforced, makes reaction feed liquid temperature control at 30-70 ℃, has the advantage that promotes the temperature control degree of accuracy in sulfamic acid production, improves the sulfamic acid yield. The production process of sulfamic acid comprises the following steps: when the special production equipment is used for producing sulfamic acid, urea is subjected to intermittent feeding and blowing feeding, so that the accurate temperature control of reaction liquid is realized, and the yield of sulfamic acid is improved.
Description
Technical Field
The application relates to the field of preparation of sulfamic acid, in particular to equipment and a process for producing sulfamic acid.
Background
Sulfamic acid is a solid strong acid, also called solid sulfuric acid, which has strong acidity, but small corrosivity, high stability, easy water solubility and wide application. Industrially, sulfamic acid is used as a descaling corrosion inhibitor, an organic synthetic sulfonating agent, an electroplating additive, a denitrating agent, a catalyst for chemical reaction and a bleaching agent in the textile industry of a heat exchange system; in agriculture, sulfamic acid is useful as a pesticide herbicide.
The large-scale production process flow of the conventional sulfamic acid comprises the following steps: adding urea and fuming sulfuric acid into a reaction kettle, stirring and mixing to dissolve the urea in the fuming sulfuric acid, and controlling the dissolving temperature to be 30-40 ℃; when the urea is completely dissolved, the reaction temperature is raised to 80-85 ℃, and the heat preservation reaction is carried out for 3-4h, thus generating crude products of sulfamic acid and carbon dioxide. The crude product is subjected to the steps of dilution, recrystallization, filtration and drying to obtain the finished product sulfamic acid with the purity of at least 99.5 percent.
The dissolution temperature of urea in oleum is an important process parameter, and when the dissolution temperature is too high, the yield of sulfamic acid is reduced for the following reasons: (1) SO contained in oleum3The reaction kettle can quickly escape, and the raw materials participating in the reaction are reduced; (2) the density of the urea is lower than that of fuming sulfuric acid, and the urea can float on the fuming sulfuric acid to react with acid mist at the top of the reaction kettle to generate SO2、CO2And the like.
However, in practical production, controlling the urea dissolution temperature is always a difficult point in process production, for the following reasons: (1) the urea has strong hygroscopicity and is easy to agglomerate, and when the urea is dissolved in fuming sulfuric acid, the local temperature of the reaction feed liquid rises suddenly, and the temperature of the reaction feed liquid is not uniform; (2) the reaction of urea with oleum is itself a violent exothermic reaction; (3) the sulfamic acid slurry prepared by the reaction has high viscosity, is difficult to dissipate heat and is difficult to cool.
At present, the control method for the urea dissolving temperature in the industry comprises the following steps: the cooling jacket is sleeved outside the reaction kettle, the coil pipe is arranged in the jacket, the coil pipe is filled with cooling liquid, the reaction kettle is cooled, and the reaction liquid and the cooling liquid indirectly exchange heat, so that the cooling rate is low, the temperature control effect is not ideal, and the yield of sulfamic acid is 83 +/-0.5%.
Disclosure of Invention
In order to improve the accuracy of temperature control in sulfamic acid production and improve the yield of sulfamic acid, the application provides equipment and a process for producing sulfamic acid.
In a first aspect, the present application provides a production apparatus for sulfamic acid, which adopts the following technical scheme:
the production equipment of sulfamic acid comprises a reaction kettle with a jacket, wherein a feeding pipeline is communicated with the reaction kettle, a hopper communicated with the feeding pipeline is arranged on the feeding pipeline, a temperature joint control assembly is arranged between the hopper and the reaction kettle and used for controlling the opening and closing of a hopper flashboard, a blower is arranged at one end, far away from the reaction kettle, of the feeding pipeline, an air outlet of the blower is communicated with the feeding pipeline, and the air supply direction of the blower is the urea feeding direction.
By adopting the technical scheme, the temperature joint control assembly is arranged between the hopper and the reaction kettle, the temperature of the reaction material liquid in the reaction kettle is monitored, when the temperature of the reaction material liquid is overhigh, the hopper gate plate is closed by the temperature joint control assembly, the feeding is stopped, the continuous heat generation in the reaction kettle is avoided from the source, and the temperature of the material liquid is controlled within the range of 30-70 ℃; meanwhile, the air flow blown in by the blower is used as a power source to convey urea on one hand, and the agglomerated urea is crushed on the other hand, so that the urea is uniformly distributed in fuming sulfuric acid when being blown into the reaction kettle, the possibility of sudden rise of the local temperature of the reaction feed liquid is reduced, the temperature control accuracy in the production of sulfamic acid is improved, and the yield of sulfamic acid is improved.
Preferably, the temperature joint control assembly comprises a temperature measuring pipe, heat-conducting insulating glue, a temperature measuring instrument, a wire and a temperature control valve, the temperature measuring pipe is located at the top of the reaction kettle, the bottom end of the temperature measuring pipe is closed, the top end of the temperature measuring pipe is communicated with the outside to form a temperature measuring cavity, the temperature measuring instrument is placed in the temperature measuring cavity, the temperature measuring pipe is filled with the heat-conducting insulating glue, the temperature measuring instrument is immersed in the heat-conducting insulating glue, the temperature control valve is used for controlling the opening and closing of the hopper gate, and the wire is connected with the temperature measuring instrument and.
Through adopting above-mentioned technical scheme, the cooperation of thermoscope and temperature-sensing valve is used in the accuse subassembly is united to the temperature, and the temperature that the thermoscope recorded transmits to the temperature-sensing valve, and opening and close of temperature-sensing valve control hopper flashboard carries out intermittent type nature reinforced, and when the upper limit value that the temperature of reaction feed liquid exceeded the temperature-sensing valve and sets up, in time cut off the urea pay-off, reduces the temperature of reaction feed liquid, realizes carrying out accurate control to the reaction feed liquid temperature.
Preferably, one end of the feeding pipeline, which is far away from the blower, is inserted into the bottom of the reaction kettle.
Through adopting above-mentioned technical scheme, in the feeding pipe inserts reation kettle, on the one hand, the direct reaction feed liquid that gets into of hair-dryer air current, promote the disturbance of reaction feed liquid, make reaction heat distribution even, the cooling rate of reaction feed liquid is very fast, on the other hand, because the air current temperature is less than reaction feed liquid temperature, the air current produces the heat exchange with the reaction feed liquid, the heat of partial reaction feed liquid is taken away when the air current rises, improve the cooling rate of reaction feed liquid, thereby make the temperature stability of reaction feed liquid in suitable scope, the sulfamic acid finished product yield has been improved.
Preferably, one end of the feeding pipeline inserted into the reaction kettle is U-shaped.
Through adopting above-mentioned technical scheme, the pipeline that feeds that the U type set up makes urea carry out the secondary crushing when carrying, further improves the dispersion degree of urea in fuming sulfuric acid, improves the control accuracy of reaction feed liquid temperature.
Preferably, reation kettle top fixedly connected with electric mixer, electric mixer includes fixed connection at the motor at reation kettle top, rotates the (mixing) shaft of being connected with the motor, be equipped with a plurality of paddles on the (mixing) shaft.
Through adopting above-mentioned technical scheme, the paddle sets up a plurality ofly, on the one hand, increases the fluidic disorderly degree in reation kettle for urea evenly distributed is in fuming sulfuric acid, concentrates when avoiding urea and fuming sulfuric acid to dissolve and releases heat, and on the other hand makes reaction feed liquid fully contact with the air current, carries out rapid cooling, improves temperature control's the degree of accuracy, increases sulfamic acid yield.
In a second aspect, the present application provides a process for producing sulfamic acid, which is implemented in the aforementioned production facility for sulfamic acid, comprising the steps of:
(1) injecting fuming sulfuric acid into the reaction kettle, wherein the fuming sulfuric acid contains SO3 20-60wt%；
(2) Adding oleum under stirringHeating to 30 deg.C, simultaneously starting the blower, and controlling the blower at 1000-3Blowing urea into the reaction kettle along a feeding pipeline at the airflow speed of/h;
(3) in the urea feeding process, the opening and closing of the hopper flashboard are controlled by the temperature joint control assembly, when the temperature of the reaction feed liquid is higher than 70 ℃, the hopper flashboard is closed by the temperature joint control assembly, feeding is suspended, when the temperature of the reaction feed liquid is 30-70 ℃, the hopper flashboard is opened by the temperature joint control assembly, feeding is continued, and after the urea feeding is finished, the blower is closed; controlling the mass ratio of the total amount of the added urea to the fuming sulfuric acid to be 1: (6.0-6.5);
(4) heating to raise the temperature of the reaction liquid to 80-85 ℃, keeping the temperature and reacting for 2-4h to prepare sulfamic acid slurry, and sequentially diluting, separating and purifying the sulfamic acid slurry to obtain a finished product of sulfamic acid.
By adopting the technical scheme, the production equipment for producing the sulfamic acid is used for producing, and the temperature of the reaction feed liquid is accurately controlled, so that the yield of the sulfamic acid is improved to 89.1 percent from 82.7 percent.
Preferably, the oleum concentration is SO-containing3 20-30wt%。
Through adopting above-mentioned technical scheme, the concentration and the viscosity of oleum are directly proportional, and the viscosity that reduces oleum can make the reaction feed liquid descend, makes the urea dissolve fast in oleum on the one hand, and on the other hand, lower viscosity can promote the heat exchange of outer air current and reaction feed liquid in the reation kettle for cooling rate, thereby improve the degree of accuracy of reaction feed liquid temperature control, improve the productivity of sulfamic acid.
Preferably, the air flow rate of the blower in the step 2 is 1400-1600m3/h。
By adopting the technical scheme, if the flow velocity of the air flow is small, the disturbance effect on the reaction feed liquid is poor, the cooling rate of the reaction feed liquid is slow, and the accuracy of the temperature control of the reaction feed liquid is weakened; if the flow velocity of the air flow is high, the reaction slurry in the reaction kettle splashes, the wall of the reaction kettle is impacted at a high speed, and the production safety is reduced; within the flow velocity range of the air flow, the disturbance effect on the reaction slurry is better on the premise of ensuring the safety of the production of the sulfamic acid, and the yield of the sulfamic acid is improved from 89.1 percent to 91.6 percent.
Preferably, the stirring speed in the step 2 is controlled to be 300-500 r/min.
By adopting the technical scheme, the urea dissolution rate is higher when the stirring rate is controlled within the range, but the temperature change range of the reaction feed liquid is still between 30 and 70 ℃, and the influence on the yield of the sulfamic acid is little.
Preferably, when the sulfamic acid slurry is diluted in the step 4, the volume ratio of the sulfamic acid slurry to the water is 1 (1.1-1.3), and the sulfamic acid slurry is discharged from the reaction kettle and injected into the water.
By adopting the technical scheme, the sulfamic acid is added into water for dilution, and the dilution temperature of the sulfamic acid can be controlled, so that the hydrolysis rate of the sulfamic acid is reduced in the dilution process of the sulfamic acid, and the yield of the sulfamic acid is improved.
In summary, the present application has the following beneficial effects:
1. because temperature joint controller and hair-dryer cooperation use in the production facility of this application, the input mode of urea is that the clearance nature is reinforced and the pay-off of blowing, promotes the degree of accuracy of temperature control in the sulfamic acid production, improves the productivity of sulfamic acid.
2. According to the method, the accurate temperature control of the reaction liquid is realized through the special production equipment for sulfamic acid, so that the temperature of the reaction liquid is maintained in a stable range when urea is dissolved, and the productivity of sulfamic acid is improved.
Drawings
FIG. 1 is a block diagram of the equipment for carrying out the sulfonation reaction of the process of the present application.
Reference numerals: 1. a reaction kettle; 11. an acid injection pipeline; 12. an exhaust gas conduit; 13. a feed line; 14. a steam line; 15. a discharge pipeline; 2. a jacket; 21. a circulating coolant line; 3. an electric mixer; 31. a paddle; 4. a hopper; 5. a blower; 6. a temperature joint control component; 61. a temperature measuring tube; 62. heat-conducting insulating glue; 63. a temperature measuring instrument; 64. a wire; 65. a temperature control valve.
Detailed Description
Preparation example of Heat-conductive insulating paste
Preparation example
The heat-conducting insulating glue is prepared by the following preparation steps:
p1, weighing 100g of polyethylene glycol with the average molecular weight of 600, adding 3.0g of silicon nitride powder with the average particle size of 0.6 mu m, and performing ultrasonic dispersion with the ultrasonic frequency of 50Hz and the ultrasonic time of 1h to prepare polyethylene glycol-silicon nitride suspension;
adding 110g of TDI and 0.3g of benzoyl chloride into the P2 and polyethylene glycol-silicon nitride suspension, uniformly stirring, heating to 75 ℃, reacting for 1h under heat preservation, and defoaming for 2h under vacuum to obtain the heat-conducting insulating adhesive.
Examples
An sulfamic acid production facility of the present application is described in further detail below with reference to figure 1:
referring to fig. 1, the production equipment of sulfamic acid comprises a reaction kettle 1, wherein the top of the reaction kettle 1 is communicated with an acid injection pipeline 11, and fuming sulfuric acid is injected into the reaction kettle 1 through the acid injection pipeline 11.
Referring to fig. 1, 1 top fixedly connected with electric mixer 3 of reation kettle, electric mixer 3 is including fixing the motor at 1 top of reation kettle, rotate the (mixing) shaft of being connected with the motor, the (mixing) shaft inserts reation kettle 1 in, be equipped with a plurality of paddles 3 on the (mixing) shaft, electric mixer 3's motor drive (mixing) shaft, the (mixing) shaft drives paddle 31 rotatory, a plurality of paddles 31 can improve the interior material disorder degree of reation kettle 1, promote the evenly distributed of material in reation kettle 1.
Referring to fig. 1, a feeding pipeline 13 is arranged at the top of a reaction kettle 1, the feeding pipeline 13 is composed of a horizontal section and a vertical section, the vertical section is communicated with the horizontal section, the horizontal section of the feeding pipeline 13 extends out of the reaction kettle 1, the vertical section is positioned in the reaction kettle 1, a hopper 4 is arranged on the horizontal section feeding pipeline 13, the hopper 4 is used for storing urea, the bottom of the hopper 4 is communicated with the horizontal section feeding pipeline 13, the urea falls into the horizontal section feeding pipeline 13 from the bottom of the hopper 4, a blower 5 is arranged at one end of the horizontal section feeding pipeline 13 far away from the reaction kettle 1, an air blowing port of the blower 5 is communicated with the horizontal section feeding pipeline 13, the blower 5 blows air to the urea feeding direction, the urea falls into the horizontal section feeding pipeline 13 vertically, the horizontal air flow blows off the urea, the blown off urea impacts on the pipe wall at the communication position of the horizontal section and the, the primary crushed urea is blown by an air stream into a vertical section feeding pipe 13.
Referring to fig. 1, the one end that vertical section conveying pipeline 13 is close to reation kettle 1 bottom is the U type, U type opening is towards reation kettle 1 top, the U type sets up and makes the broken urea of once carry out the secondary crushing in the air current turning, further improves the dispersion degree of urea, urea after the secondary crushing is blown in reation kettle 1 by the air current, dissolve in fuming sulfuric acid, the urea of less granularity makes reaction feed liquid temperature more even, avoid the abrupt rise of reaction feed liquid temperature, improve temperature control's the degree of accuracy.
Referring to fig. 1, a temperature joint control assembly 6 is arranged between a hopper 4 and a reaction kettle 1, the temperature joint control assembly 6 comprises a temperature measuring tube 61, a heat-conducting insulating adhesive 62, a temperature measuring instrument 63, a lead wire 64 and a temperature control valve 65, the temperature measuring tube 61 is positioned at the top of the reaction kettle 1, the bottom end of the temperature measuring tube 61 is closed, the top end of the temperature measuring tube 61 is communicated with the outside to form a temperature measuring cavity, the temperature measuring instrument 63 is placed in the temperature measuring cavity to measure the temperature of reaction liquid in the reaction kettle 1, the heat-conducting insulating adhesive 62 prepared by the preparation example is injected into the temperature measuring tube 61 until the temperature measuring instrument 63 is immersed, the heat-conducting insulating adhesive 62 is solidified to fix the position of the temperature measuring instrument 63 in the temperature measuring cavity, the hopper 4 valve is the temperature control valve 65, the temperature control valve 65 is used for controlling the opening and closing of the hopper 4 shutter, the lead wire 64 is electrically connected with the, the temperature control valve 65 receives a temperature signal to control the opening and closing of the gate of the hopper 4, when the temperature measured by the temperature measuring instrument 63 exceeds 70 ℃, the temperature control valve 65 drives the gate of the hopper 4 to be closed, and when the temperature measured by the temperature measuring instrument 63 is 30-70 ℃, the temperature control valve 65 drives the gate of the hopper 4 to be opened, so that the linkage control of the temperature of the reaction feed liquid and the feeding amount of urea is realized, and the accuracy of the reaction temperature control is improved.
Referring to fig. 1, a circulating cooling liquid pipeline 21 is arranged in an outer jacket 2 of a reaction kettle 1, the pipe wall of the circulating cooling liquid pipeline 21 is abutted against the outer wall of the reaction kettle 1, liquid in the circulating cooling liquid pipeline 21 is petroleum ether with the temperature of 0 ℃, and the petroleum ether circularly flows from bottom to top in the circulating cooling liquid pipeline 21 to cool reaction liquid.
Referring to fig. 1, when heating is required in reaction vessel 1, steam pipe 14 at the top of reaction vessel 1 transmits steam into reaction vessel 1, so as to realize the heating function of reaction vessel 1.
Referring to fig. 1, an exhaust gas pipe 12 at the top of the reaction vessel 1 balances the pressure in the reaction vessel 1, thereby improving the production safety.
Application example
Application example 1
A process for producing sulfamic acid, which is carried out in the sulfamic acid production facility described in the examples, comprising the steps of:
s1, preparation of sulfamic acid slurry:
opening an acid injection pipeline of oleum, and injecting 500kg oleum into the reaction kettle at one time, wherein the oleum contains SO360wt%, starting the electric stirrer, wherein the stirring speed is 500r/min, opening a steam pipeline and a thermodetector, introducing steam, and closing the steam pipeline when the temperature of fuming sulfuric acid is 30 ℃;
adding 81kg urea into a hopper, opening a temperature control valve and a blower, and adjusting the airflow flow of the blower to 1000m3Adjusting the opening of a hopper gate plate to enable the feeding rate of urea to be 9 kg/h;
when the temperature of the reaction feed liquid measured by the temperature measuring instrument exceeds 70 ℃, the temperature control valve drives the hopper gate plate to close, the urea feeding is suspended, and when the temperature of the reaction feed liquid measured by the temperature measuring instrument is 30-70 ℃, the temperature control valve drives the hopper gate plate to open;
starting a circulating cooling pipeline while starting the blower, and circularly introducing petroleum ether at the temperature of 0 ℃ for cooling;
after the urea is fed, closing the blower, opening the steam pipeline again, directly introducing steam, heating the mixture to the temperature of 80-85 ℃, and carrying out heat preservation reaction for 2 hours to obtain sulfamic acid reaction slurry;
s2, preparation of crude sulfamic acid: injecting water into a dilution tank to enable the volume ratio of the water to the sulfamic acid reaction slurry to be 1:1.1, adding the sulfamic acid reaction slurry under the stirring condition, diluting for the first time, cooling by using a jacket in the dilution process, controlling the temperature of a dilution feed liquid to be 20-50 ℃, stopping stirring after the reaction slurry is added, standing and settling for 4 hours, opening a siphon valve, starting a siphon pump, removing the upper layer of diluted acid in the dilution tank, starting a stirrer after the siphon is finished, adding a dilution liquid into the dilution tank again for the second dilution, stopping stirring after the dilution liquid is added, standing and settling for 4 hours, filtering for the first time by using a bag filter, wherein the solid obtained by filtering is a sulfamic acid crude product, the filtrate is a primary filtering mother liquor, and the dilution liquid is formed by mixing the mother liquor and the sulfamic acid crude product according to the volume ratio of 1: 0.1;
s3, purification of sulfamic acid: dissolving the crude sulfamic acid product in a dissolving kettle, adding water, stirring until the refined sulfamic acid solution is supersaturated, indirectly heating a jacket of the dissolving kettle, heating to 68-72 ℃, cooling for crystallization, performing secondary filtration by using a bag filter, wherein the filtered solid is refined sulfamic acid granules, the filtrate is secondary filtered mother liquor, washing the refined sulfamic acid granules with water, filtering by using the bag filter, and drying the filtered solid in a dryer to obtain the finished product sulfamic acid with the yield of 89.1% and the purity of 99.8%.
Application examples 2 to 4
A process for producing sulfamic acid, which is operated on the basis of application example 1, and is different from application example 1 in that: the added oleum has different concentrations:
| application example | Oleum concentration (containing SO)3Mass fraction of (2) | Yield (%) | Purity (%) |
| Application example 2 | 30wt% | 90.1 | 99.8 |
| Application example 3 | 25wt% | 90.4 | 99.6 |
| Application example 4 | 20wt% | 90.3 | 99.7 |
Application examples 5 to 8
A process for producing sulfamic acid, which is operated on the basis of application example 3, and is different from application example 3 in that: the air flow speed of the added blower is different:
| application example | Velocity of air flow (m)3/h） | Yield (%) | Purity (%) |
| Application example 5 | 1400 | 90.7 | 99.8 |
| Application example 6 | 1500 | 91.2 | 99.7 |
| Application example 7 | 1600 | 91.6 | 99.7 |
| Application example 8 | 2000 | 89.7 | 99.5 |
Comparative application example
Comparative application example 1
A method for producing sulfamic acid, which is similar to the operation steps of the application example 1 and is different from the application example 1 in that: in the step 3, urea feeding equipment and feeding modes are different, the bottom of the hopper is communicated with the top of the reaction kettle, urea is fed into the reaction kettle at one time, the temperature control assembly and the blower are closed between the hopper and the reaction kettle, and finally the yield of the finished sulfamic acid product is 82.7 percent, and the purity is 99.5 percent.
Comparative application example 2
A method for producing sulfamic acid, which is similar to the operation steps of the application example 1 and is different from the application example 1 in that: in the step 3, urea feeding equipment and feeding modes are different, the bottom of a hopper is communicated with the top of a reaction kettle, a temperature control assembly which is the same as that in the embodiment is arranged between the hopper and the reaction kettle, when the temperature of reaction feed liquid measured by a temperature measuring instrument exceeds 70 ℃, a temperature control valve drives a hopper flashboard to close, urea feeding is suspended, when the temperature of reaction feed liquid measured by the temperature measuring instrument is 30-70 ℃, the temperature control valve drives the hopper flashboard to open, and finally, the yield of the finished sulfamic acid product is 86.3%, and the purity is 99.6%.
Comparative application example 3
A method for producing sulfamic acid, which is similar to the operation steps of the application example 1 and is different from the application example 1 in that: in the step 3, in the urea feeding link, different urea feeding modes are adopted, a blower is started to blow and feed, the temperature joint control assembly is closed, urea is continuously fed, and finally the yield of the sulfamic acid finished product is 85.4% and the purity is 99.6%.
Data analysis
As can be seen from the yields of the application example 1 and the comparative application example 1, urea is added at one time and is not crushed before being added, when the urea is dissolved in fuming sulfuric acid, the temperature of the reaction feed liquid is reduced by only a cooling jacket, the temperature control effect of the reaction feed liquid is poor, and the yield is reduced from 89.1% to 82.7%, so that the temperature control accuracy can be remarkably improved by the matched use of the temperature joint control component and the blower, the temperature of the reaction feed liquid is stabilized at 30-70 ℃, and the yield of sulfamic acid is improved.
From the yields of application example 1 and comparative application examples 1 to 2, it was found that the temperature control effect was weaker than that of the case where the temperature joint control unit and the blower were used in combination, and the yield was reduced from 89.1% to 86.3%, although the intermittent feeding was carried out only by using the temperature joint control unit, which was effective in controlling the temperature of the reaction feed liquid.
From the yields of application example 1 and comparative application example 3, it can be seen that the temperature control effect of the reaction feed liquid is poor and the yield of urea is reduced from 89.1% to 85.4% by feeding only with a blower to crush the agglomerated urea, and feeding the urea continuously.
From the sulfamic acid yields in application examples 1 to 4, it can be seen that when oleum contains SO3 When the concentration is 25wt%, the reaction liquid is cooled quickly due to moderate viscosity, and the urea dissolution rate is high, so that the optimum fuming sulfuric acid concentration in the sulfamic acid production is obtained.
From the results of application example 3 and application examples 5 to 8, it was found that the air flow speed of the hair dryer was 1600m3And in the hour, the removal rate of the water in the urea is high, and the disturbance on the reaction liquid is good on the premise of safe production, so that the optimal airflow speed in the production of the sulfamic acid is obtained.
In conclusion, the temperature joint control component and the blower have a synergistic effect in the aspect of controlling the reaction temperature, and the temperature control accuracy is obviously improved by using the temperature joint control component and the blower in a matched manner, so that the yield of sulfamic acid is obviously improved; meanwhile, the best production method of sulfamic acid comprises the following steps: the production method of example 7 was applied.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The production equipment of sulfamic acid comprises a reaction kettle (1) with a jacket (2), wherein the reaction kettle (1) is communicated with a feeding pipeline (15), and is characterized in that: the feeding pipeline (13) is provided with a hopper (4) communicated with the feeding pipeline, a temperature joint control assembly (6) is arranged between the hopper (4) and the reaction kettle (1), the temperature joint control assembly (6) is used for controlling the opening and closing of a gate plate of the hopper (4), one end, away from the reaction kettle (1), of the feeding pipeline (13) is provided with a blower (5), an air outlet of the blower (5) is communicated with the feeding pipeline (13), and the air supply direction of the blower (5) is the urea feeding direction.
2. The production facility of sulfamic acid according to claim 1, characterized in that: the temperature joint control assembly (6) comprises a temperature measuring tube (61), heat-conducting insulating glue (62), a temperature measuring instrument (63), a lead (64) and a temperature control valve (65); the temperature measuring pipe (61) is located in the reaction kettle (1), the bottom end of the temperature measuring pipe (61) is closed, the top end of the temperature measuring pipe is communicated with the outside to form a temperature measuring cavity, the temperature measuring instrument (63) is placed in the temperature measuring cavity, heat-conducting insulating glue (62) is filled in the temperature measuring pipe (61), the temperature measuring instrument (63) is immersed in the heat-conducting insulating glue (62), the temperature control valve (65) is used for controlling the opening and closing of the gate of the hopper (4), and the lead (64) is connected with the temperature measuring instrument (63) and the temperature control valve (65).
3. A production facility of sulfamic acid according to claim 2, characterized in that: one end of the feeding pipeline (13) far away from the blower (5) is inserted into the bottom of the reaction kettle (1).
4. A production facility of sulfamic acid according to claim 3, characterized in that: one end of the feeding pipeline (13) inserted into the reaction kettle (1) is U-shaped.
5. The production facility of sulfamic acid according to claim 4, characterized in that: the reactor is characterized in that an electric stirrer (3) is fixedly connected to the top of the reactor (1), the electric stirrer (3) comprises a motor fixedly connected to the top of the reactor (1) and a stirring shaft rotatably connected with the motor, and a plurality of blades (31) are arranged on the stirring shaft.
6. A process for the production of sulfamic acid, characterized in that it is carried out in a plant for the production of sulfamic acid according to claim 1, comprising the following steps:
(1) injecting fuming sulfuric acid into the reaction kettle, wherein the fuming sulfuric acid contains SO3 20-60wt%；
(2) Heating oleum to 30 deg.C under stirring, and simultaneously starting blower, controlling the blower at 1000-3Blowing urea into the reaction kettle along a feeding pipeline at the airflow speed of/h;
(3) in the urea feeding process, the opening and closing of a hopper gate plate are controlled by a temperature joint control assembly; when the temperature of the reaction feed liquid is higher than 70 ℃, the temperature joint control assembly closes the hopper gate plate and stops feeding; when the temperature of the reaction feed liquid is 30-70 ℃, the temperature joint control assembly opens a hopper gate plate to feed; after urea feeding is finished, the blower is closed, and the mass ratio of the total amount of the fed urea to fuming sulfuric acid is controlled to be 1: (6.0-6.5);
(4) heating to raise the temperature of the reaction liquid to 80-85 ℃, keeping the temperature and reacting for 2-4h to prepare sulfamic acid slurry, and sequentially diluting, separating and purifying the sulfamic acid slurry to obtain a finished product of sulfamic acid.
7. The process according to claim 6, wherein: the oleum contains SO320-30wt%。
8. The process according to claim 7, wherein: the air flow speed of the blower in the step 2 is 1400-1600m3/h。
9. The process according to claim 8, wherein: the stirring speed in the amino step 2 is controlled to be 300-500 r/min.
10. A process according to claim 9 for the production of sulfamic acid, characterized in that: when the sulfamic acid slurry is diluted in the step 4, the volume ratio of the sulfamic acid slurry to the water is 1 (1.1-1.3), and the sulfamic acid slurry is discharged from the reaction kettle and is injected into the water.
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