CN111302316A - Method and device for continuously preparing sulfamic acid - Google Patents
Method and device for continuously preparing sulfamic acid Download PDFInfo
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- CN111302316A CN111302316A CN202010148933.0A CN202010148933A CN111302316A CN 111302316 A CN111302316 A CN 111302316A CN 202010148933 A CN202010148933 A CN 202010148933A CN 111302316 A CN111302316 A CN 111302316A
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Abstract
The invention discloses a green continuous preparation method and a device of sulfamic acid, wherein the preparation method comprises the following steps: dissolving urea in concentrated sulfuric acid, and simultaneously loading the urea and sulfur trioxide gas with the temperature of 35-45 ℃ and the volume fraction of 2-15% into an upper section of falling film reactor and a lower section of falling film reactor with different inner diameters through a gas-liquid distributor; and after the falling film reaction is finished, carrying out gas-liquid separation, emptying gas after passing through a demister, feeding the slurry after the gas-liquid separation into a solid-liquid separator, circulating concentrated sulfuric acid containing a small amount of urea obtained through the solid-liquid separation to the raw material, and feeding the obtained solid product sulfamic acid to a packaging line. The invention realizes continuous production, does not need to transport, store and measure fuming sulfuric acid and liquid sulfur trioxide which are easy to solidify, reduces manual work entering an operation area, and greatly improves the safety performance; the reaction process is close to zero emission, the atom economy is extremely high, and the method has very important application value and practical significance.
Description
Technical Field
The invention relates to a green continuous preparation method and a device of sulfamic acid, belonging to the technical field of synthesis of sulfamic acid.
Background
Sulfamic acid, also known as sulfamic acid, CAS accession No. 5329-14-6; as an important fine chemical, the metal cleaning agent is widely applied to the fields of metal cleaning, food, printing and dyeing, electroplating, papermaking and the like.
At present, the synthesis process routes of sulfamic acid at home and abroad mainly comprise: 1) carrying out solid-liquid phase reaction on urea and fuming sulfuric acid; 2) dissolving urea in an organic solvent, and adding fuming sulfuric acid to carry out liquid-liquid reaction; 3) the sulfur trioxide and ammonia gas are subjected to gas-gas reaction to produce an intermediate, and then water is added for hydrolysis. Chinese patent CN 101391759a discloses a process for solid-liquid reaction of 23% fuming sulfuric acid and urea, then adding a large amount of dilute sulfuric acid to separate sulfamic acid, the invention can produce a large amount of dilute sulfuric acid, which causes great pressure on environmental protection, and the process belongs to batch reaction, and the mass of each batch is different. Chinese patent CN105524006A discloses a process for synthesizing sulfamic acid by gas phase reaction of sulfur trioxide and ammonia gas, which can produce a large amount of ammonium sulfate by-products, and has very strict requirements on the moisture content in the reaction system and severe corrosion on equipment. Chinese patent CN1597500A discloses a process for carrying out solid-liquid reaction between a small amount of fuming sulfuric acid and urea, and then supplementing liquid sulfur trioxide for further reaction, wherein although the process slows down the intensity of the reaction to a certain extent, the liquid sulfur trioxide has strong oxidizability, the mass transfer effect in a reaction kettle is poor, a large amount of carbide can be generated locally, the temperature rises sharply to initiate the second step reaction, and a large amount of carbon dioxide escapes from the system to cause the pot to be out of danger and be extremely dangerous. In addition, fuming sulfuric acid and sulfur trioxide used for production are extremely unstable and highly corrosive dangerous chemicals, are usually solid under cold conditions, are difficult to store and have high transportation cost. Therefore, the current oleum and liquid sulfur trioxide can not meet the requirement of large-scale production no matter considering economic cost and environmental protection pressure.
Disclosure of Invention
The invention aims to provide a green, continuous and molecular economic preparation method and a device of sulfamic acid.
The invention provides a green continuous preparation method of sulfamic acid, which has the reaction principle that urea dissolved in concentrated sulfuric acid reacts with gas-phase sulfur trioxide in an equimolar way to generate an intermediate in an upper-stage falling film reactor, and when the intermediate enters a lower-stage falling film reactor, the temperature is increased, the intermediate is decomposed to generate two molecules of target products of sulfamic acid and one molecule of carbon dioxide. The reaction equation is shown as follows:
the invention provides a green continuous preparation method of sulfamic acid, which is realized by the following technical scheme and comprises the following steps:
the method comprises the following steps that sulfur dioxide and dry air are catalytically converted into sulfur trioxide in a sulfur trioxide conversion tower through a catalyst, then the sulfur trioxide is cooled to 35-50 ℃ in a pipeline and enters a sulfur trioxide filter, a small amount of contained nicotinic acid and catalyst dust are removed, sulfur trioxide gas and urea dissolved in concentrated sulfuric acid enter a gas-liquid distributor together, the temperature of the sulfur trioxide gas is 35-45 ℃, and the volume fraction of the sulfur trioxide gas is 2-15%; the distributed liquid flows down along the inner wall of the falling film reactor to form a film, the gas forms an extrusion effect on the liquid film in the center of the falling film reactor to enable the liquid film to be laminar flow or turbulent flow, the gas and the slurry are separated in a gas-liquid separator after the reaction of an upper falling film reactor and a lower falling film reactor, the gas enters a demister to remove liquid drops carried in high-speed flowing gas and then is emptied, the slurry after the gas-liquid separation enters a solid-liquid separator to be separated, the liquid obtained after the solid-liquid separation is concentrated sulfuric acid containing a small amount of unreacted urea, the concentrated sulfuric acid is recycled to a batching process before a gas-liquid distributor, and the separated solid is a target product of sulfamic acid and then is sent to.
In the method, the source of the sulfur trioxide is obtained by catalyzing sulfur dioxide with a catalyst.
In the method, the concentration of the sulfur trioxide is 2-15% by volume, the diluting gas is dry air with a dew point lower than-50 ℃, and the temperature of the diluting sulfur trioxide gas is 35-45 ℃.
In the method, the temperature of the upper-section jacket of the falling film reactor is 30-50 ℃, and the temperature of the lower-section jacket is 70-90 ℃.
The invention provides a green continuous preparation device of sulfamic acid, which comprises a sulfur trioxide conversion tower, a sulfur trioxide filter, a gas-liquid distributor, a falling film reactor, a gas-liquid separator, a demister and a solid-liquid separator which are connected in sequence;
the top of the sulfur trioxide conversion tower is provided with inlets for sulfur dioxide and dry air, and the sulfur trioxide conversion tower catalytically converts the sulfur dioxide and the dry air into sulfur trioxide; the bottom of the sulfur trioxide conversion tower is connected with a sulfur trioxide filter which removes nicotinic acid contained in sulfur trioxide; a nicotinic acid outlet is formed at the bottom of the sulfur trioxide filter, a sulfur trioxide gas outlet at the top is connected with a gas-liquid distributor, and the gas-liquid distributor distributes sulfur trioxide gas and urea dissolved in concentrated sulfuric acid so as to form a uniform film on the falling film reactor; the bottom outlet of the gas-liquid distributor is connected with a falling film reactor, the falling film reactor is an upper falling film reactor and a lower falling film reactor with different inner diameters, the inner diameter of the lower section is larger than that of the upper section, urea and sulfur trioxide in the upper section react to form an intermediate, and the lower section is used for decomposing the intermediate; the bottom of the falling film reactor is connected with a gas-liquid separator, and the gas-liquid separator separates the reacted slurry from gas; a gas outlet of the gas-liquid separator is connected with a demister, and a liquid outlet of the gas-liquid separator is connected with a solid-liquid separator; the demister is used for separating liquid drops carried in gas after gas-liquid separation; and the solid-liquid separator is used for separating the slurry into a target product of sulfamic acid and a concentrated sulfuric acid solution containing a small amount of unreacted urea, and the concentrated sulfuric acid solution separated from the solid-liquid separator flows back to the batching process before the gas-liquid distributor.
In the device, the falling film reactor is two sections of falling film reactors with different inner diameters, the inner diameter of the lower section is larger than that of the upper section, the inner diameter of the upper section is 6-25mm and 1-10m long, and the inner diameter of the lower section is 8-30mm and 1-6m long.
In the device, the gas-liquid separator is a cyclone separator or a baffling separator.
In the device, the solid-liquid separator is a centrifuge or a plate-and-frame filter press.
The invention has the beneficial effects that:
the invention provides a method for preparing sulfamic acid, which has the advantages of low production cost, no waste acid, high safety performance, continuous production and basic realization of atom economic reaction. The method has the advantages that the reaction equipment occupies small area, the equipment is not corroded in the production process, the mass transfer and heat transfer efficiency of the falling film reactor is high, the product conversion rate is high, the number of byproducts is small, and the yield of the target product is higher than 95%; the method has the advantages that the method does not need to use a solvent, is simple in post-treatment, and better in product quality, the excessive sulfuric acid is still concentrated sulfuric acid which can be recycled, waste acid, waste gas and waste residue are not generated, the method is green and environment-friendly, and the production cost advantage is obvious; the falling film type reactor is used, urea, concentrated sulfuric acid and sulfur trioxide simultaneously enter the reactor, back mixing does not exist, continuous production is realized, fuming sulfuric acid and liquid sulfur trioxide which are easy to solidify are not required to be transported, stored and metered, manual entering into an operation area is reduced, and safety performance is greatly improved; the reaction system only contains reaction raw materials of urea, sulfuric acid and sulfur trioxide, basically realizes the reaction of 1:1:1, is close to zero emission, has extremely high atom economy and has very important application value and practical significance.
Drawings
FIG. 1 is a schematic view of a continuous production apparatus for sulfamic acid according to the present invention
In the figure: 1-dry air, 2-sulfur dioxide, 3-sulfur trioxide conversion tower, 4-sulfur trioxide filter, 5-nicotinic acid, 6-upper-section jacket outlet of a falling film reactor, 7-gas-liquid distributor, 8-falling film reactor, 9-lower-section jacket outlet of the falling film reactor, 10-upper-section jacket inlet of the falling film reactor, 11-lower-section jacket inlet of the falling film reactor, 12-gas-liquid separator, 13-liquid phase system of urea and concentrated sulfuric acid, 14-demister, 15-solid-liquid separator and 16-sulfamic acid packaging line.
Detailed Description
The present invention is further illustrated by, but is not limited to, the following examples.
As shown in fig. 1, the green continuous preparation device of sulfamic acid comprises a sulfur trioxide conversion tower 3, a sulfur trioxide filter 4, a gas-liquid distributor 7, a falling film reactor 8, a gas-liquid separator 12, a demister 14 and a solid-liquid separator 15 which are connected in sequence. The connection sequence is as shown in figure 1, the top of a sulfur trioxide conversion tower 3 is provided with inlets for sulfur dioxide 2 and dry air 3, and the sulfur trioxide conversion tower catalytically converts the sulfur dioxide and the dry air into sulfur trioxide; the bottom of the sulfur trioxide conversion tower 3 is connected with a sulfur trioxide filter 4, and the sulfur trioxide filter removes nicotinic acid contained in sulfur trioxide; a nicotinic acid outlet is arranged at the bottom of the sulfur trioxide filter 4, and a sulfur trioxide gas outlet at the top is connected with a gas-liquid distributor 7 which distributes sulfur trioxide gas and urea dissolved in concentrated sulfuric acid so as to form a uniform film on the falling film reactor; an outlet at the bottom of the gas-liquid distributor 7 is connected with a falling film reactor 8, urea and sulfur trioxide react to form an intermediate in the upper section of the falling film reactor, and the intermediate is decomposed in the lower section; the bottom of the falling film reactor 8 is connected with a gas-liquid separator 12, and the gas-liquid separator separates the reacted slurry from gas; a gas outlet of the gas-liquid separator 12 is connected with a demister 14, and a liquid outlet is connected with a solid-liquid separator 15; the demister is used for separating liquid drops carried in gas after gas-liquid separation; and the solid-liquid separator is used for separating the slurry into a target product of sulfamic acid and a concentrated sulfuric acid solution containing a small amount of unreacted urea, and the concentrated sulfuric acid solution separated from the solid-liquid separator returns to the batching process before the gas-liquid distributor 7.
Further, the falling film reactor is an upper falling film reactor and a lower falling film reactor with different inner diameters, the inner diameter of the lower section is larger than that of the upper section, the inner diameter of the upper section of the falling film reactor is 6-25mm and the length of the upper section of the falling film reactor is 1-10m, and the inner diameter of the lower section of the falling film reactor is 8-30mm and the length of the lower section of the falling film reactor is 1-6 m.
The gas-liquid separator is a cyclone separator or a baffling separator.
The solid-liquid separator is a centrifuge or a plate-and-frame filter press.
The continuous preparation process of the device is as follows:
Further, the molar ratio of urea to concentrated sulfuric acid is 1.0: 1.5-2.5, and the molar ratio of urea to sulfur trioxide is 1.0: 1.02-1.1.
The sulfur trioxide is obtained by catalyzing sulfur dioxide with a catalyst.
The gas for diluting sulfur trioxide is dry air with a dew point lower than minus 50 ℃, and the temperature of the diluted sulfur trioxide gas is 35-45 ℃.
Example 1
6000g of urea and 15000g of 98% sulfuric acid are uniformly mixed at room temperature, the mixed solution and 35 ℃ sulfur trioxide gas with the volume fraction of 5% and the volume fraction of 46.1L/min enter a first section of falling film reactor with the length of 1.8m and the inner diameter of 8mm at the speed of 21g/min, and the temperature of a jacket of the first section of falling film reactor is adjusted to 35 ℃; the length of the second stage falling film reactor is 1.2m, the inner diameter is 10mm, and the temperature of the jacket is 75 ℃; after cyclone separation, tail gas is evacuated after passing through a demister, a solid product obtained after reactants enter a centrifugal machine for separation is sulfamic acid, and the content of the sulfamic acid is determined to be 97.6%.
Example 2
6000g of urea and 18000g of 98 percent sulfuric acid are uniformly mixed at room temperature, 40 ℃ sulfur trioxide gas with the volume fraction of 4 percent and the rate of 72g/min and 176.4L/min enters a first section of falling film type reactor with the length of 2.5m and the inner diameter of 10mm, and the temperature of a jacket of the first section of falling film type reactor is adjusted to be 40 ℃; the length of the second stage falling film reactor is 2m, the inner diameter is 12mm, and the temperature of the jacket is 80 ℃; after baffling separation, the tail gas is evacuated after passing through a demister, reactants enter a plate frame for filter pressing separation to obtain a solid product, namely sulfamic acid, and the content of the sulfamic acid is determined to be 98.1%.
Example 3
6000g of urea and 20000g of 98 percent sulfuric acid are uniformly mixed at room temperature, and the mixture and 241.9L/min of 45 ℃ sulfur trioxide gas with the volume fraction of 8 percent enter a first section of falling film reactor with the length of 5m and the inner diameter of 14mm at the speed of 130g/min, and the temperature of a jacket of the first section of falling film reactor is adjusted to 35 ℃; the length of the second stage falling film reactor is 3 m, the inner diameter is 16mm, and the temperature of the jacket is 85 ℃; after cyclone separation, tail gas is evacuated after passing through a demister, reactants enter a plate frame for filter pressing separation, and the obtained solid product is sulfamic acid, and the content of the sulfamic acid is determined to be 96.1%.
Example 4
6000g of urea and 22000g of 98 percent sulfuric acid are uniformly mixed at room temperature, and the mixture and 45 ℃ sulfur trioxide gas with 246.4L/min and 10 percent of volume fraction enter a first section of falling film reactor with the length of 8m and the inner diameter of 14mm at the speed of 280g/min, and the temperature of a jacket of the first section of falling film reactor is adjusted to 35 ℃; the length of the second stage falling film reactor is 4m, the inner diameter is 16mm, and the temperature of the jacket is 85 ℃; after baffling separation, the tail gas is evacuated after passing through a demister, the solid product obtained after the reactant enters a centrifugal machine for separation is sulfamic acid, and the content of the sulfamic acid is determined to be 96.9%.
Example 5
6000g of urea and 25000g of 98% sulfuric acid are uniformly mixed at room temperature, 35 ℃ sulfur trioxide gas with the volume fraction of 4% and the volume fraction of 907.2L/min and the speed of 465g/min enters a first section of falling film reactor with the length of 10m and the inner diameter of 22mm, and the temperature of a jacket of the first section of falling film reactor is adjusted to 45 ℃; the length of the second stage falling film reactor is 6m, the inner diameter is 24mm, and the temperature of the jacket is 85 ℃; after cyclone separation, tail gas is evacuated after passing through a demister, a solid product obtained after reactants enter a centrifugal machine for separation is sulfamic acid, and the content of the sulfamic acid is determined to be 98.9%.
Example 6
6000g of urea and 25000g of 98% sulfuric acid are uniformly mixed at room temperature, 40 ℃ sulfur trioxide gas with the volume fraction of 2% and the volume fraction of 1251.9L/min and the speed of 341g/min enters a first section of falling film reactor with the length of 10m and the inner diameter of 25mm, and the temperature of a jacket of the first section of falling film reactor is adjusted to be 50 ℃; the length of the second stage falling film reactor is 6m, the inner diameter is 30mm, and the temperature of the jacket is 90 ℃; after cyclone separation, tail gas is evacuated after passing through a demister, reactants enter a plate frame for filter pressing separation, and the obtained solid product is sulfamic acid, and the content of the sulfamic acid is determined to be 97.2%.
Claims (8)
1. A continuous process for the preparation of sulfamic acid, characterized in that it comprises the following steps:
sulfur dioxide and dry air are catalytically converted into sulfur trioxide in a sulfur trioxide conversion tower through a catalyst, then the sulfur trioxide is cooled to 35-50 ℃ in a pipeline, the sulfur trioxide enters a sulfur trioxide filter, a small amount of contained nicotinic acid and catalyst dust are removed, sulfur trioxide gas and urea dissolved in concentrated sulfuric acid enter a gas-liquid distributor together, the distributed liquid forms a film along the inner wall of a falling film reactor and flows downwards, the gas forms an extrusion effect on a liquid film in the center of the falling film reactor, the liquid film is laminar flow or turbulent flow, after the reaction of an upper section of the falling film reactor and a lower section of the falling film reactor, a reaction system enters a gas-liquid separator to separate gas and slurry, the gas enters a demister to remove liquid drops carried in high-speed flowing gas, the slurry enters a solid-liquid separator to be separated, the separated liquid is the concentrated sulfuric acid containing a small amount of unreacted urea, and, the separated solid is the target product sulfamic acid.
2. The continuous production method of sulfamic acid according to claim 1, characterized in that: the molar ratio of urea to concentrated sulfuric acid is 1.0: 1.5-2.5, and the molar ratio of urea to sulfur trioxide is 1.0: 1.02-1.1.
3. The continuous production method of sulfamic acid according to claim 1, characterized in that: the sulfur trioxide is obtained by catalyzing sulfur dioxide with a catalyst.
4. The continuous production method of sulfamic acid according to claim 1, characterized in that: the sulfur trioxide is used after being diluted, the diluting gas is dry air with the dew point lower than minus 50 ℃, and the temperature of the diluting sulfur trioxide gas is 35-45 ℃;
the temperature of the sulfur trioxide gas entering the falling film reactor is 35-45 ℃ and the volume fraction is 2-15%.
5. A continuous production apparatus for sulfamic acid for carrying out the green continuous production method of sulfamic acid according to any one of claims 1 to 4, characterized in that:
the device comprises a sulfur trioxide conversion tower, a sulfur trioxide filter, a gas-liquid distributor, a falling film reactor, a gas-liquid separator, a demister and a solid-liquid separator which are connected in sequence;
the top of the sulfur trioxide conversion tower is provided with inlets for sulfur dioxide and dry air, and the sulfur trioxide conversion tower catalytically converts the sulfur dioxide and the dry air into sulfur trioxide; the bottom of the sulfur trioxide conversion tower is connected with a sulfur trioxide filter which removes nicotinic acid contained in sulfur trioxide; a nicotinic acid outlet is formed at the bottom of the sulfur trioxide filter, a sulfur trioxide gas outlet at the top is connected with a gas-liquid distributor, and the gas-liquid distributor distributes sulfur trioxide gas and urea dissolved in concentrated sulfuric acid so as to form a uniform film on the falling film reactor; the bottom outlet of the gas-liquid distributor is connected with a falling film reactor, the falling film reactor is an upper falling film reactor and a lower falling film reactor with different inner diameters, the inner diameter of the lower section is larger than that of the upper section, urea and sulfur trioxide in the upper section react to form an intermediate, and the lower section is used for decomposing the intermediate; the bottom of the falling film reactor is connected with a gas-liquid separator, and the gas-liquid separator separates the reacted slurry from gas; a gas outlet of the gas-liquid separator is connected with a demister, and a liquid outlet of the gas-liquid separator is connected with a solid-liquid separator; the demister separates liquid drops carried in the gas after gas-liquid separation; and the solid-liquid separator is used for separating the slurry into a target product of sulfamic acid and a concentrated sulfuric acid solution containing a small amount of unreacted urea, and the concentrated sulfuric acid solution separated from the solid-liquid separator is returned to the gas-liquid distributor for recycling in the batching process.
6. The continuous production apparatus of sulfamic acid according to claim 5, characterized in that: the inner diameter of the upper section of the falling film reactor is 6-25mm, the length of the falling film reactor is 1-10m, and the inner diameter of the lower section of the falling film reactor is 8-30mm, and the length of the falling film reactor is 1-6 m.
7. The continuous production apparatus of sulfamic acid according to claim 5, characterized in that: the gas-liquid separator is a cyclone separator or a baffling separator.
8. The continuous production apparatus of sulfamic acid according to claim 5, characterized in that: the solid-liquid separator is a centrifuge or a plate-and-frame filter press.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112694422A (en) * | 2021-01-14 | 2021-04-23 | 中国日用化学研究院有限公司 | Green continuous preparation method and device for joint production of dinonyl naphthalene disulfonic acid and alkyl benzene sulfonic acid |
| CN113401883A (en) * | 2021-07-12 | 2021-09-17 | 田雨 | Continuous reaction process and continuous reaction equipment for sulfamic acid |
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| GB965380A (en) * | 1962-02-19 | 1964-07-29 | Allied Chem | Production of sulphamic acid |
| CN1597500A (en) * | 2003-09-18 | 2005-03-23 | 铜陵化学工业集团有限公司 | Two-step preparation technology of amino sulfonic acid |
| CN104262212A (en) * | 2014-10-28 | 2015-01-07 | 湖南立新环保科技发展有限公司 | Method for continuously preparing 2,6-dinonyl naphthalene sulfonic acid |
| CN108586296A (en) * | 2018-05-16 | 2018-09-28 | 中国日用化学研究院有限公司 | A kind of method for continuously synthesizing of sodium p-nitrotoluene-2-sulfonic acid |
| CN110745796A (en) * | 2019-10-24 | 2020-02-04 | 宣城市楷昂化工有限公司 | Technology for producing sulfamic acid by using byproduct waste sulfuric acid |
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2020
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| GB965380A (en) * | 1962-02-19 | 1964-07-29 | Allied Chem | Production of sulphamic acid |
| CN1597500A (en) * | 2003-09-18 | 2005-03-23 | 铜陵化学工业集团有限公司 | Two-step preparation technology of amino sulfonic acid |
| CN104262212A (en) * | 2014-10-28 | 2015-01-07 | 湖南立新环保科技发展有限公司 | Method for continuously preparing 2,6-dinonyl naphthalene sulfonic acid |
| CN108586296A (en) * | 2018-05-16 | 2018-09-28 | 中国日用化学研究院有限公司 | A kind of method for continuously synthesizing of sodium p-nitrotoluene-2-sulfonic acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112694422A (en) * | 2021-01-14 | 2021-04-23 | 中国日用化学研究院有限公司 | Green continuous preparation method and device for joint production of dinonyl naphthalene disulfonic acid and alkyl benzene sulfonic acid |
| CN113401883A (en) * | 2021-07-12 | 2021-09-17 | 田雨 | Continuous reaction process and continuous reaction equipment for sulfamic acid |
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