CN112678783A - Preparation system and method of calcium thiosulfate solution - Google Patents
Preparation system and method of calcium thiosulfate solution Download PDFInfo
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Abstract
The invention relates to a preparation system and a preparation method of a calcium thiosulfate solution, belonging to the technical field of chemical fertilizer preparation, wherein the raw materials are an ammonium thiosulfate solution and calcium hydroxide, and the ammonium thiosulfate solution and the calcium hydroxide are subjected to a replacement reaction at a certain temperature and stirring speed to prepare the calcium thiosulfate solution; the reaction temperature is 70-85 ℃; the stirring speed is 60-80 rpm. The preparation method of the calcium thiosulfate solution has the advantages of high production efficiency, low equipment investment cost, high production safety coefficient, yield of over 94 percent and good product quality.
Description
Technical Field
The invention relates to a preparation system and a preparation method of a calcium thiosulfate solution, and belongs to the technical field of fertilizer preparation.
Technical Field
The calcium thiosulfate solution is used as an agricultural fertilizer to supplement calcium and sulfur elements for crops, and can also be used as a treating agent and a loosening agent for soil acidification and hardening, wherein the calcium element is completely soluble in water, the calcium content is higher than 6%, and the effectiveness is greatly higher than that of calcium products such as gypsum powder and shell sintering (the calcium element of the products is only about 5% soluble in water).
U.S. Pat. No. 2012/0031158A1 discloses a synthetic route for the production of a calcium thiosulfate solution: preparing calcium hydroxide slurry by combining calcium oxide and water, adding sulfur into the calcium hydroxide slurry, reacting the sulfur and the calcium hydroxide to form a reaction mixture, adding an oxidant into the reaction mixture to obtain a suspension, adding acid into the suspension, adding a flocculating agent into the suspension, and recovering the calcium thiosulfate solution.
CaO+H2O→Ca(OH)2
3Ca(OH)2+6S→2CaS2+CaS2O3+3H2O
4Ca(OH)2+8S→2CaS3+CaS2O3+3H2O+Ca(OH)2
5Ca(OH)2+10S→2CaS4+CaS2O3+3H2O+2Ca(OH)2
2CaS2+CaS2O3+3O2→3CaS2O3
The synthesis method needs to be carried out in high pressure of 10-15 atmospheres, has high pressure resistance requirement on production equipment, needs more equipment, has high production safety risk, complex process and low efficiency, and simultaneously produces products with higher pH value and needs a large amount of acid for adjustment, thereby causing high overall production cost.
Therefore, the development of a preparation system and a preparation method of a calcium thiosulfate solution with high production efficiency, low equipment investment cost, high production safety coefficient, high yield (more than 94%) and good product quality is a technical problem which needs to be solved urgently in the technical field.
Disclosure of Invention
One of the purposes of the invention is to develop a preparation system of the calcium thiosulfate solution, which has the advantages of high production efficiency, low equipment investment cost, high production safety coefficient, high yield (more than 94 percent) and good product quality.
The above object of the present invention is achieved by the following technical solutions:
a preparation system of a calcium thiosulfate solution comprises a calcium thiosulfate reaction unit, an ammonia gas absorption unit, a tail gas absorption unit and an ammonia gas reaction unit; the calcium thiosulfate reaction unit is connected with the ammonia absorption unit through a pipeline, the ammonia absorption unit is connected with the tail gas absorption unit through a pipeline, and the ammonia absorption unit and the tail gas absorption unit are respectively connected with the ammonia reaction unit through pipelines.
Preferably, the calcium thiosulfate reaction unit comprises a reaction device, a stirring device and a condensing device; the stirring device is positioned in the reaction device, and the condensing device is positioned at the periphery of the reaction device.
Preferably, the ammonia gas absorption unit comprises a primary absorption device, a secondary absorption device and a tertiary absorption device; the first-stage absorption device is respectively connected with the second-stage absorption device and the third-stage absorption device through pipelines, and the second-stage absorption device is connected with the third-stage absorption device through pipelines.
Preferably, the tail gas absorption unit comprises a tower body, a filler supporting and compacting device, a liquid and gas distributor, a liquid distributor and a tower top spraying device.
Preferably, the ammonia reaction unit comprises a reaction device, a stirring device and a condensing device; the stirring device is positioned in the reaction device, and the condensing device is positioned at the periphery of the reaction device.
Preferably, the calcium thiosulfate reaction unit is connected with the ammonia absorption unit through a pipeline and a condensing device.
Preferably, the tertiary absorption device in the ammonia absorption unit is connected with the tail gas absorption unit through a vacuum pump.
Preferably, the tail gas absorption unit is connected with the ammonia reaction unit through a pump.
Preferably, the tertiary absorption device in the ammonia gas absorption unit is connected with the ammonia gas reaction unit through a pump.
Preferably, the ammonia reaction unit is connected with the calcium thiosulfate reaction unit through a pipeline.
The invention also aims to develop a preparation method of the calcium thiosulfate solution, which has the advantages of high production efficiency, low equipment investment cost, high production safety coefficient, high yield (more than 94 percent) and good product quality.
The above object of the present invention is achieved by the following technical solutions:
a process for preparing the solution of calcium thiosulfate includes such steps as preparing the solution of ammonium thiosulfate and calcium hydroxide, and displacement reaction at a certain temp and stirring speed.
Preferably, the ammonia gas is used to produce ammonium thiosulfate.
Preferably, the reaction equation is as follows:
(NH4)2S2O3+Ca(OH)2＝CaS2O3+NH3+H2O。
preferably, the ammonium thiosulfate solution has a concentration of 26% to 60%, photographic grade.
Preferably, the molar ratio of ammonium thiosulfate to calcium hydroxide is 1.00: 1.00-1.05: 1.00.
preferably, the reaction temperature is 70-85 ℃.
Preferably, the stirring speed is 60 to 80 rpm.
Preferably, the concentration of the calcium thiosulfate solution is more than or equal to 24 percent, and the calcium content is more than or equal to 6.3 percent.
Has the advantages that:
the preparation system and the preparation method of the calcium thiosulfate solution have the advantages of high production efficiency, low equipment investment cost, high production safety coefficient, yield of over 94 percent and good product quality.
The invention is further illustrated by the following figures and specific examples, which are not meant to limit the scope of the invention.
Drawings
FIG. 1 is a schematic view of the structure of a system for producing a calcium thiosulfate solution of the present invention.
Names of main parts:
1 tail gas absorption tower 2 vacuum pump
3 three-stage absorption tank and 4 two-stage absorption tank
5 first-stage absorption tank 6 condenser
78 ammonia reation kettle of reation kettle
Detailed Description
Unless otherwise stated, the raw materials in the examples of the present invention are conventional raw materials available on the market, the equipment used is equipment commonly used in the art, and the reaction conditions are normal conditions; the identification of the product is identified by conventional methods.
Example 1: the mol ratio of ammonium thiosulfate to calcium hydroxide is 1.00: 1.00, the reaction temperature is 80 +/-2 ℃, the reaction time is 5 hours, and the stirring speed is 60 revolutions per minute.
FIG. 1 is a schematic view showing the structure of a system for producing a calcium thiosulfate solution according to the present invention; wherein, 1 is a tail gas absorption tower, 2 is a vacuum pump, 3 is a three-stage absorption tank, 4 is a two-stage absorption tank, 5 is a one-stage absorption tank, 6 is a condenser, 7 is a reaction kettle, and 8 is an ammonia reaction kettle; the preparation system of the calcium thiosulfate solution comprises: the system comprises a tail gas absorption tower 1, a vacuum pump 2, a three-stage absorption tank 3, a two-stage absorption tank 4, a one-stage absorption tank 5, a condenser 6, a reaction kettle 7 and an ammonia reaction kettle 8; the reaction kettle 7 comprises a reaction kettle body, a stirrer and a condenser, wherein the stirrer is positioned in the kettle body, the condenser is positioned at the periphery of the reaction kettle body, the top of the reaction kettle 7 is connected with the top of the primary absorption tank 5 through the condenser 6 and a pipeline, and a raw material inlet at the top of the reaction kettle 7 is connected with an ammonia reaction kettle 8 through a pipeline (not shown in the figure) and used for putting ammonium thiosulfate; the top of the primary absorption tank 5 is connected with the secondary absorption tank 4 through a pipeline; the top of the first-stage absorption tank 5 is connected with the third-stage absorption tank 3 through a pipeline (not shown in the figure), and the bottom of the first-stage absorption tank 5 is connected with the top of the ammonia reaction kettle 8 through a pipeline; the secondary absorption tank 4 is connected with the tertiary absorption tank 3 through a pipeline; the third-stage absorption tank 3 is connected with the middle part of the tail gas absorption tower 1 through a vacuum pump 2; the bottom of the tail gas absorption tower 1 is connected with an ammonia absorption unit through a pump and a pipeline and the top of an ammonia reaction kettle 8. The tail gas absorption unit comprises a tower body, a filler supporting and pressing device, a liquid and gas distributor, a liquid distributor and a tower top spraying device.
The preparation method of the calcium thiosulfate solution comprises the following steps:
(1) preparation of ammonium thiosulfate solution
The ammonium thiosulfate solution is photographic grade, the content of the ammonium thiosulfate solution can be used when the ammonium thiosulfate solution is more than 26 percent, the required amount of the ammonium thiosulfate solution is calculated according to the molar ratio of the ammonium thiosulfate solution to the calcium hydroxide and the volume of the reaction kettle, the calculation is carried out by combining the target content requirement of the calcium thiosulfate with the content of more than or equal to 24 percent, when the content of the used ammonium thiosulfate is more than 26 percent, required quantitative water is added, but the content of the ammonium thiosulfate in the aqueous solution added into the reaction kettle is required to be ensured to be more than or equal to.
(2) The ammonium thiosulfate solution reacts with calcium hydroxide
Taking a three-cube reaction kettle as an example, selecting a commercially available photographic-grade ammonium thiosulfate solution (the content is about 57 percent generally), firstly adding water into the reaction kettle (the water adding amount is determined according to the content of the ammonium thiosulfate, and the aim is to control the content of the ammonium thiosulfate in the liquid in the kettle to be about 26 percent), then adding 332 kg of calcium hydroxide (the mass requirement of the calcium hydroxide is that the content of heavy metals is less than 5ppm calculated by lead, and the content of lead, chromium, arsenic and mercury is less than 1ppm and the content of iron is less than 50ppm respectively), sealing the reaction kettle, starting stirring (the stirring speed is controlled at 60 rpm), starting a vacuum system for about 10 minutes, sucking the ammonium thiosulfate solution by using the vacuum system, wherein the adding amount of the ammonium thiosulfate is 665 kg, starting to heat when the vacuum degree is about-0.03, and keeping the temperature to 80 +/-2 ℃ for 5 hours. The reaction process is accompanied by a large amount of ammonia gas to be discharged, the absorption system can absorb more than 95 percent of ammonia gas, the rest part of ammonia gas is absorbed by the tail gas absorption system, and the ammonia water with the concentration of about 8 percent generated in the absorption system can be recycled and used as a raw material for producing the ammonium thiosulfate solution and can also be used as a raw material for other tail gas absorption liquid containing sulfur dioxide. After the reaction is finished, a circulating water cooling system is started to cool down to about 40 ℃.
(3) Product handling
And (3) central control analysis: after the reaction of the calcium hydroxide and the ammonium thiosulfate solution is finished and the temperature is reduced to about 40 ℃, taking a 400 ml sample, filtering to obtain a colorless, clear and transparent solution, detecting the pH value (within the range of 7.0-9.0) at 25 ℃, detecting the specific gravity at 25 ℃ to be more than 1.245, and detecting the content of the calcium thiosulfate by an iodine titration method to be more than 24.5 percent, wherein the calcium hydroxide and the ammonium thiosulfate solution are considered to be normal and can be further processed into finished products.
And (3) filtering: and (3) carrying out vacuum filtration on the finished product, namely a coarse filtration process, filtering obvious unreacted slag and unreacted slag in the calcium hydroxide to obtain turbid coarse filtrate, and then carrying out fine filtration on the turbid coarse filtrate by using a plate and frame filter to obtain colorless, clear and transparent liquid.
And (3) confirmation of the product: the calcium content is about 6.4 percent according to NYT 1117-2010 detection, the calcium thiosulfate content is 24.5 percent, the specific gravity is 1.245 according to GB/T4472-2011 detection, the PH value is between 8.00 +/-1.00 according to GB/T9724-2007 detection, the lead chromium-arsenic-mercury content is respectively less than 1ppm according to GB/T30902-2014, ammonia gas is generated by using ammonium thiosulfate as a main raw material and reacting at the same time, and the nitrogen content is below 0.1 percent (the content can be used as a nitrogen fertilizer in a liquid fertilizer and has no side effect) according to GB/T8572-2010 detection.
Example 2: the mol ratio of ammonium thiosulfate to calcium hydroxide is 1.05: 1.00, the reaction temperature is 70 +/-3 ℃, the reaction time is 6 hours, and the stirring speed is 70 r/m.
The preparation method of the calcium thiosulfate solution comprises the following steps:
(1) preparation of ammonium thiosulfate solution
The ammonium thiosulfate solution is photographic, water is added to prepare the ammonium thiosulfate solution with the content of 30%, and the calculation is carried out by combining the requirement that the target content of the calcium thiosulfate is more than or equal to 27%.
(2) The ammonium thiosulfate solution reacts with calcium hydroxide
Taking a three-cube reaction kettle as an example, selecting a commercially available photographic-grade ammonium thiosulfate solution (the general content is about 57%), firstly adding water into the reaction kettle (the water adding amount is determined according to the content of the ammonium thiosulfate, and the aim is to control the content of the ammonium thiosulfate in the liquid in the kettle to be 30%), then adding 332 kg of calcium hydroxide (the quality requirement of the calcium hydroxide is that the content of heavy metals is less than 5ppm calculated on lead, and the content of lead, chromium, arsenic and mercury is respectively required to be less than 1ppm and the content of iron is less than 50ppm), sealing the reaction kettle, starting stirring (the stirring speed is controlled at 70 r/min) for about 10 minutes, starting a vacuum system, sucking the ammonium thiosulfate solution by using the vacuum system, wherein the adding amount of the ammonium thiosulfate is 698 kg, starting to heat up when the vacuum degree is about-0.03, the temperature rises to 70 ℃ until the reaction time is 6 hours. The reaction process is accompanied by a large amount of ammonia gas to be discharged, the absorption system can absorb more than 95 percent of ammonia gas, the rest part of ammonia gas is absorbed by the tail gas absorption system, and the ammonia water with the concentration of about 8 percent generated in the absorption system can be recycled and used as a raw material for producing the ammonium thiosulfate solution and can also be used as a raw material for other tail gas absorption liquid containing sulfur dioxide. After the reaction is finished, a circulating water cooling system is started to cool down to about 40 ℃.
(3) Product handling
And (3) central control analysis: after the reaction of the calcium hydroxide and the ammonium thiosulfate solution is finished and the temperature is reduced to about 40 ℃, taking a 400 ml sample, filtering to obtain a colorless, clear and transparent solution, detecting that the pH value at 25 ℃ is within the range of 8.00 +/-1.00, detecting that the specific gravity at 25 ℃ is more than 1.280, and detecting that the content of the calcium thiosulfate is more than 27%, wherein the calcium hydroxide and the ammonium thiosulfate are considered to be normal and can be further processed into finished products.
And (3) filtering: and (3) carrying out vacuum filtration on the finished product, namely a coarse filtration process, filtering obvious unreacted slag and unreacted slag in the calcium hydroxide to obtain turbid coarse filtrate, and then carrying out fine filtration on the turbid coarse filtrate by using a plate and frame filter to obtain colorless, clear and transparent liquid.
And (3) confirmation of the product: the calcium content is more than 7.0 percent and the reduced content of calcium thiosulfate is more than 27 percent according to NYT 1117-.
Example 3: the mol ratio of ammonium thiosulfate to calcium hydroxide is 1.02: 1.00, the reaction temperature is 85 +/-3 ℃, the reaction time is 4 hours, and the stirring speed is 80 r/min.
The preparation method of the calcium thiosulfate solution comprises the following steps:
(1) preparation of ammonium thiosulfate solution
The ammonium thiosulfate solution is photographic, water is added to prepare the ammonium thiosulfate solution with the content of 26%, and the calculation is carried out by combining the requirement that the target content of the calcium thiosulfate is more than or equal to 24.5%.
(2) The ammonium thiosulfate solution reacts with calcium hydroxide
Taking a three-cube reaction kettle as an example, selecting a commercially available photographic-grade ammonium thiosulfate solution (the general content is about 57%), firstly adding water into the reaction kettle (the water addition amount is determined according to the content of the ammonium thiosulfate, and the aim is to control the content of the ammonium thiosulfate in the liquid in the kettle to be 26%), then adding 332 kg of calcium hydroxide (the quality requirement of the calcium hydroxide is that the content of heavy metals is less than 5ppm calculated on lead, and the content of lead, chromium, arsenic and mercury is respectively required to be less than 1ppm and the content of iron is less than 50ppm), sealing the reaction kettle, starting stirring (the stirring speed is controlled at 80 revolutions per minute) for about 10 minutes, starting a vacuum system, sucking the ammonium thiosulfate solution by using the vacuum system, adding the ammonium thiosulfate in an amount of 678.3 kg, starting to heat up when the vacuum degree is about-0.03, raising the temperature to 70 ℃, reacting for 4 hours, and discharging a large amount of ammonia gas in the reaction process, the absorption system can absorb more than 95% of ammonia gas, the rest is absorbed by the tail gas absorption system, and the ammonia water which is about 8% and is generated in the tail gas absorption system can be recycled and used as raw materials for producing ammonium thiosulfate solution, and can also be used as raw materials of other tail gas absorption liquid containing sulfur dioxide. After the reaction is finished, a circulating water cooling system is started to cool down to about 40 ℃.
(3) Product handling
And (3) central control analysis: after the reaction of the calcium hydroxide and the ammonium thiosulfate solution is finished and the temperature is reduced to about 40 ℃, taking a 400 ml sample, filtering to obtain a colorless, clear and transparent solution, detecting that the pH value at 25 ℃ is in the range of 8.00 +/-1.00, detecting that the specific gravity at 25 ℃ is more than 1.260, and detecting that the content of the calcium thiosulfate is more than 24.5%, wherein the calcium hydroxide and the ammonium thiosulfate are normal and can be further processed into finished products.
And (3) filtering: and (3) carrying out vacuum filtration on the finished product, namely a coarse filtration process, filtering obvious unreacted slag and unreacted slag in the calcium hydroxide to obtain turbid coarse filtrate, and then carrying out fine filtration on the turbid coarse filtrate by using a plate and frame filter to obtain colorless, clear and transparent liquid.
And (3) confirmation of the product: the calcium content is detected according to NYT 1117-2010 and is more than 6.3 percent, the reduced calcium sulfate content is more than 24.5 percent, the specific gravity is detected according to GB/T4472-2011 and is about 1.255, the pH value is detected according to GB/T9724-2007 and is between 7.0 and 9.0, the lead-chromium-arsenic-mercury content is respectively less than 1ppm according to GB/T30902-2014, and as the ammonium thiosulfate is used as a main raw material and reacts to generate ammonia gas, certain residue exists in the solution, and the nitrogen content is detected according to GB/T8572-2010 and is generally 0.3 percent (the nitrogen fertilizer can be used as a nitrogen fertilizer in the liquid fertilizer, and the content has no side effect).
The preparation method of the calcium thiosulfate solution provided by the invention bypasses the problems of high reaction conditions, such as high pressure and long reaction time, which are required by direct synthesis, and adopts a simpler replacement reaction, namely a reaction mechanism of gas generation and strong base-to-weak base preparation, so that the reaction is simple and easy to implement.
Claims (10)
1. A preparation system of a calcium thiosulfate solution is characterized in that: the device comprises a calcium thiosulfate reaction unit, an ammonia gas absorption unit, a tail gas absorption unit and an ammonia gas reaction unit; the calcium thiosulfate reaction unit is connected with the ammonia absorption unit through a pipeline, the ammonia absorption unit is connected with the tail gas absorption unit through a pipeline, and the ammonia absorption unit and the tail gas absorption unit are respectively connected with the ammonia reaction unit through pipelines.
2. The system for preparing a calcium thiosulfate solution according to claim 1, characterized in that: the calcium thiosulfate reaction unit comprises a reaction device, a stirring device and a condensing device; the stirring device is positioned in the reaction device, and the condensing device is positioned at the periphery of the reaction device.
3. The system for preparing a calcium thiosulfate solution according to claim 2, characterized in that: the ammonia gas absorption unit comprises a primary absorption device, a secondary absorption device and a tertiary absorption device; the first-stage absorption device is respectively connected with the second-stage absorption device and the third-stage absorption device through pipelines, and the second-stage absorption device is connected with the third-stage absorption device through pipelines.
4. The system for preparing a calcium thiosulfate solution according to claim 3, characterized in that: the tail gas absorption unit comprises a tower body, a filler supporting and pressing device, a liquid and gas distributor, a liquid distributor and a tower top spraying device.
5. The system for preparing a calcium thiosulfate solution according to claim 4, characterized in that: the ammonia reaction unit comprises a reaction device, a stirring device and a condensing device; the stirring device is positioned in the reaction device, and the condensing device is positioned at the periphery of the reaction device.
6. The system for preparing a calcium thiosulfate solution according to claim 5, characterized in that: the device comprises a thiocalcium sulfate reaction unit, a tail gas absorption unit, a tertiary absorption device, a pump, an ammonia reaction unit and a condensing device, wherein the thiocalcium sulfate reaction unit is connected with the ammonia absorption unit through a pipeline and the condensing device, the tertiary absorption device in the ammonia absorption unit is connected with the tail gas absorption unit through the vacuum pump, the tail gas absorption unit is connected with the ammonia reaction unit through the pump, the tertiary absorption device in the ammonia absorption unit is connected with the ammonia reaction unit through the pump, and the ammonia reaction unit is connected with the thiocalcium sulfate reaction.
7. A preparation method of a calcium thiosulfate solution comprises the following steps: the raw materials are ammonium thiosulfate solution and calcium hydroxide, and the replacement reaction is carried out at a certain reaction temperature and stirring speed to prepare calcium thiosulfate solution;
the reaction equation is as follows:
(NH4)2S2O3+Ca(OH)2＝CaS2O3+NH3+H2O；
the reaction temperature is 70-85 ℃; the stirring speed is 60-80 rpm.
8. The method for preparing a calcium thiosulfate solution according to claim 7, characterized in that: the concentration of the ammonium thiosulfate solution is 26-60%.
9. The method for preparing a calcium thiosulfate solution according to claim 8, characterized in that: the molar ratio of the ammonium thiosulfate to the calcium hydroxide is 1.00: 1.00-1.05: 1.00.
10. the method for preparing a calcium thiosulfate solution according to claim 9, characterized in that: the concentration of the calcium thiosulfate solution is more than or equal to 24 percent.
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