CN215626832U - Processing apparatus of ammonium chloride waste liquid in industrial-grade glycine production - Google Patents
Processing apparatus of ammonium chloride waste liquid in industrial-grade glycine production Download PDFInfo
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Abstract
The utility model relates to a treatment device of ammonium chloride waste liquid in industrial glycine production, wherein a film evaporator is connected with an extraction kettle through a material transfer pump; the feed inlet of the extraction kettle is respectively connected with a solvent pipeline, a concentrate pipeline, a solvent reflux pipeline, an extraction condenser and a centrifugal filtrate circulating pipe, the outlet of the extraction kettle is connected with a centrifuge, and the jacket of the extraction kettle is connected with circulating water; the top of the single-effect heater is connected with the gas-phase rectifying tower through a Roots blower, and the lower part of the single-effect heater is connected with the secondary evaporation tank through a material transfer pump; the upper part of the secondary evaporation tank is respectively connected with the evaporation tank, the preheater and the secondary evaporation condenser, and the lower part of the secondary evaporation tank is connected with the organic matter tank. The recovered ammonium chloride can be mixed with normal ammonium chloride as a byproduct in the production of glycine for taking out, and the organic matter solution can be taken out to organic fertilizer enterprises to be mixed with yeast solution for large-scale use. The device can realize high-valued comprehensive utilization of the ammonium chloride waste liquid, does not generate waste water, can finally realize zero clearing of the red waste liquid in the glycine industry, and has remarkable environmental protection benefit.
Description
Technical Field
The utility model discloses a treatment device for ammonium chloride waste liquid in industrial glycine production, belongs to the technical field of chemical production, and particularly relates to a treatment device for ammonium chloride waste liquid in a glycine production process by a chloroacetic acid ammonolysis method.
Background
Currently, the traditional chloroacetic acid ammonolysis process is still adopted in domestic industrial-grade glycine production, and the process can be simply described as follows: reacting chloroacetic acid aqueous solution with ammonia under the catalysis of urotropine, and then extracting by adopting methanol, crystallizing, centrifuging and drying to obtain a glycine product; the centrifuged methanol mother liquor is sequentially subjected to methanol rectification, double-effect countercurrent and flash evaporation concentration, cooling crystallization, thickening and centrifugation to obtain a yellow byproduct ammonium chloride which is used for producing a fertilizer and simultaneously generates a large amount of red waste liquor. The process has many defects, such as low yield, unrecoverable catalyst urotropine, complex chemical reaction caused by high-temperature rectification, high COD evaporated condensed water generation, difficult-to-treat red waste liquid and the like, and the treatment of the red waste liquid becomes the biggest pain point of glycine enterprises.
The final red waste liquor in glycine production essentially consists of: 34.6% of ammonium chloride, 50% of water, 14% of ammonium dichloroacetate, 6.2% of urotropine, 1% of glycine, 3.2% of ammonium acetate, 3% of iminodiacetic acid, 1% of methanol esters and the like. Disc granulation or drum granulation is generally adopted in the industry, the waste liquid is used for producing chlorine-based organic fertilizer, biological bacterial fertilizer, organic-inorganic compound fertilizer and the like, but because the fertilizer industry has strict requirements on indexes such as chloride ions, total nutrients, organic matters, moisture, pH and the like, the use amount of the waste liquid is small, the release of glycine capacity is influenced to a greater or lesser extent, legal utilization can not be achieved, and environmental protection risks exist.
Disclosure of Invention
The utility model provides a treatment device for ammonium chloride waste liquid in industrial glycine production, which can recover an ammonium chloride product from a red waste liquid byproduct in glycine production and simultaneously produce an organic solution, wherein the ammonium chloride can be mixed with normal ammonium chloride in glycine production for selling, and the organic solution can be sold to organic fertilizer enterprises for being mixed with yeast liquid for large-scale use.
In order to realize the purpose of the utility model, the following technical scheme is adopted, which comprises the following structures:
a treatment device for ammonium chloride waste liquid in industrial glycine production is characterized in that a film evaporator is connected with an extraction kettle through a material transfer pump;
the outlet of the extraction kettle is connected with a bag-pulling type centrifuge;
the bag-pulling type centrifuge is connected with a centrifugal filtrate tank, the centrifugal filtrate tank is connected with a single-effect heater, and the single-effect heater is connected with a single-effect evaporation tank;
the bottom of the single-effect evaporation tank is connected with a secondary evaporation tank, and the secondary evaporation tank is connected with an organic matter tank.
The top of the single-effect evaporation tank is connected with the gas-phase rectifying tower; the top of the gas-phase rectifying tower is sequentially connected with a first-stage condenser and a second-stage condenser, the second-stage condenser is connected with a solvent storage tank, and the solvent storage tank is connected with the gas-phase rectifying tower.
The bottom of the gas phase rectifying tower is connected with a reboiler, the reboiler is connected with a secondary evaporation water supplementing tank, and the secondary evaporation water supplementing tank is connected with a preheater.
The preheater is connected with the secondary evaporating pot, and the secondary evaporating pot is connected with the organic matter tank.
The top of the secondary evaporation tank is connected with a secondary evaporation primary condenser and a secondary evaporation secondary condenser in turn through steam pipelines and then is connected with a dilute solvent tank.
A hot water tank inlet pipe is further arranged at the bottom of the secondary evaporation tank, the hot water tank is connected with a dryer, and the dryer is connected with the hot water tank to form a circulation loop; the top of the secondary evaporation tank is also connected with a dryer through a steam pipeline.
The treatment process of the ammonium chloride waste liquid in the industrial glycine production by adopting the device comprises the following steps:
dehydrating the ammonium chloride waste liquid by a thin film evaporator to form concentrated jelly, adding a solvent into an extraction kettle to dissolve organic substances in the jelly, extracting ammonium chloride, and filtering out a crude product of the ammonium chloride by a bag-type centrifuge;
buffering filtrate from the bag-pulling type centrifuge by a centrifugal filtrate tank, continuously feeding the filtrate into a single-effect heater and a single-effect evaporation tank for forced circulation concentration, further purifying most of solvent vapor generated by the single-effect evaporation tank, and feeding heavy components extracted from the bottom of the single-effect evaporation tank into a secondary evaporation tank;
the solvent vapor from the top of the single-effect evaporation tank is further concentrated by a rectification system of a gas-phase rectification tower, a reboiler and a solvent reflux tank, and then is condensed and recovered by a first-stage condenser and a second-stage condenser to obtain a purified solvent which can be directly used; heavy components (the temperature is higher than 80 ℃, most of the water) at the bottom of the gas-phase rectifying tower can be directly used as water supplement of the secondary evaporation tank after being condensed by the preheater;
heavy components extracted from the bottom of the single-effect evaporation tank enter a secondary evaporation tank for heating and concentrating, a dilute solvent is obtained by condensation of a secondary evaporation primary condenser and a secondary evaporation secondary condenser, and the dilute solvent enters the gas-phase rectifying tower again for purification after being preheated by a preheater;
the solution which can not be concentrated in the secondary evaporation tank is the organic solution product.
The ammonium chloride waste liquid comprises 15-20% of ammonium chloride, 40-60% of moisture, 10-18% of ammonium dichloroacetate, 4-8% of urotropine, 0.5-2% of glycine, 1-5% of ammonium acetate, 1-5% of iminodiacetic acid and 0.5-2% of lipid substances, wherein the lipid substances comprise methyl carbinol, acetic ester and methyl chloroacetate; the ammonium chloride waste liquid is concentrated until the water content is below 30 percent before being added into a mixed solvent for dissolution.
The mixed solvent comprises one or more of methanol, ethanol, propanol, butanol, isopropanol, isobutanol, n-butanol, acetone, butanone, formic acid, methylal and acetic acid, and the weight ratio of the concentrate to the mixed solvent is controlled to be 0.5-4.
The vacuum degree in the reduced pressure distillation process is-0.07 to-0.09 Mpa, and the temperature is 50 to 70 ℃.
The utility model has simple structure, can realize high-valued comprehensive utilization of the ammonium chloride waste liquid, generates no waste water, generates economic benefit, can finally realize zero clearing of the red waste liquid in the glycine industry, and has obvious environmental protection benefit and economic benefit.
Drawings
Fig. 1 is a schematic structural diagram 1 of a treatment device for ammonium chloride waste liquid in industrial-grade glycine production.
Fig. 2 is a schematic structural diagram 2 of a treatment device for ammonium chloride waste liquid in industrial-grade glycine production.
Fig. 3 is a schematic structural diagram 3 of a treatment device for ammonium chloride waste liquid in industrial-grade glycine production.
Wherein, 1, a film evaporator, 2, an extraction kettle, 3, an extraction condenser, 4, a bag-pulling type centrifuge, 5, a centrifugal filtrate tank, 6, a single-effect heater, 7, a single-effect evaporation tank, 8, a gas-phase rectification tower, 9, a reboiler, 10, a primary condenser, 11, a secondary condenser, 12, a solvent storage tank, 13, a secondary evaporation water-supplementing tank, 14, a preheater, 15, a secondary evaporation tank, 16, an organic matter tank, 17, a hot water tank, 18, a dryer, 19, a secondary evaporation primary condenser, 20, a secondary evaporation secondary condenser, 21, a dilute solvent tank, 22, a water circulation vacuum pump, 2-1, an ammonium chloride solution concentrate pipeline, 2-2, a solvent pipeline, 2-3, a solvent condensate pipeline, 2-4, an extraction kettle tail gas pipeline, 2-5, an extraction liquid discharge pipeline, 4-1, a centrifugal filtrate pipeline, 5-1 part of a filtrate extraction pipeline, 5-2 parts of a filtrate return administration, 5-3 parts of a single-effect evaporation feeding pipeline, 7-1/7-2/7-3 parts of a single-effect evaporation circulating pipe, 8-1 part of a rectifying tower gas-phase feeding pipeline, 8-3/8-4 parts of a rectifying tower and reboiler circulating pipeline, 10-1 parts of a solvent gas-phase pipe, 14-1 parts of a secondary evaporation tank water replenishing pipeline, 7-4 parts of a single-effect concentrated solution extraction pipeline, 13-1 parts of a rectifying tower kettle water pipeline, 15-1 parts of a solvent gas-phase pipe, 16-1 parts of an organic matter loading pipeline, 17-1 parts of a hot water pipeline, 18-1 parts of a solvent gas-phase pipe, 18-2 parts of an ammonium chloride product discharge, 19-1 parts of a solvent gas-phase pipe, 20-1 parts of a vacuum pipeline, 21-1, dilute solvent extraction line.
Detailed Description
Example 1
Fig. 1, 2 and 3, wherein fig. 1, 2 and 3 are a series of process routes, which are only arranged separately. Each device is provided with a pipeline, the specific pipeline names being as explained in the description of the figures.
A treatment device for ammonium chloride waste liquid in industrial glycine production is characterized in that a film evaporator 1 is connected with an extraction kettle 2 through an ammonium chloride solution concentrate pipeline 2-1 and a transfer pump;
the outlet of the extraction kettle 2 is connected with a bag-pulling type centrifuge 4; an extraction condenser is arranged at the top of the extraction kettle 2.
The centrifuge 4 is connected with a centrifugal filtrate tank 5, the centrifugal filtrate tank 5 is connected with a single-effect heater 6, and the single-effect heater 6 is connected with a single-effect evaporation tank 7;
the bottom of the single-effect evaporation tank 7 is connected with a secondary evaporation tank 15, and the secondary evaporation tank 15 is connected with an organic matter tank 16.
The top of the single-effect heater 7 is connected with a gas-phase rectifying tower 8; the top of the gas-phase rectifying tower 8 is sequentially connected with a first-stage condenser 10 and a second-stage condenser 11, the second-stage condenser 11 is connected with a solvent storage tank 12, and the solvent storage tank 12 is connected with the gas-phase rectifying tower 8.
The bottom of the gas phase rectifying tower 8 is connected with a reboiler 9, the reboiler 9 is connected with a secondary evaporation water supplementing tank 13, and the secondary evaporation water supplementing tank 13 is connected with a preheater 14.
The preheater 14 is connected with the secondary evaporation tank 15, and the secondary evaporation tank 15 is connected with the organic matter tank 16.
The top of the secondary evaporation tank 15 is connected with a secondary evaporation primary condenser 19 and a secondary evaporation secondary condenser 20 in sequence through steam pipelines and then connected with a dilute solvent tank 21.
The bottom of the secondary evaporation tank 15 is also provided with a hot water tank 17 inlet pipe, the hot water tank 17 is connected with a dryer 18, and the dryer 18 is connected with the hot water tank 17 to form a circulation loop; the top of the secondary evaporation tank 15 is also connected with a dryer 18 through a steam pipeline.
Example 2
At 6.25m3Feed rate/h into the thin film evaporator Red waste stream (17.5% ammonium chloride, 51.2% moisture, 11.8% ammonium dichloroacetate, 5.6% urotropin, 1.5% glycine, 3.5% ammonium acetate, 4.3% iminodiacetic acid, 1.6% lipids including methyl carbinol, acetate, methyl chloroacetate), thin film evaporatorThe temperature is controlled to be about 80 ℃, the vacuum degree is controlled to be-0.07 to-0.09 Mpa, and the concentrate with certain viscosity (the water content is 28.1 percent, the chlorine content is 24.9 percent, the total nitrogen content is 16.3 percent, and the organic matter content is 25.6 percent) is produced.
4000kg of concentrate is added into a K8000L enamel reaction kettle through a screw pump, 710L of methylal and 3000L of isopropanol are added, after stirring for 2h, 723kg of ammonium chloride is filtered out by a centrifuge. The centrifuged filtrate was subjected to reduced pressure distillation to recover a solvent mixture (methylal and isopropanol), and then 200L of water was added thereto, followed by reduced pressure distillation to obtain 2390kg of an organic matter solution, and the analytical data: the water content is 19.5%, the total nitrogen content is 7.7%, the chlorine content is 9.3%, the organic matter content is 40.7%, and the fluidity is good (the viscosity at 30 ℃ is 98 cP).
Example 3
At 6.25m3The red waste liquid (17.5 percent of ammonium chloride, 51.2 percent of moisture, 11.8 percent of ammonium dichloroacetate, 5.6 percent of urotropine, 1.5 percent of glycine, 3.5 percent of ammonium acetate, 4.3 percent of iminodiacetic acid and 1.6 percent of lipid substances are fed into the film evaporator, wherein the lipid substances comprise methyl carbinol, acetate and methyl chloroacetate), the temperature of the film evaporator is controlled to be about 80 ℃, the vacuum degree is controlled to be-0.07 to-0.09 Mpa, and the concentrate with high viscosity (the moisture content is 28.1 percent, the chlorine content is 24.9 percent, the total nitrogen content is 16.3 percent and the organic matter content is 25.6 percent) is produced.
4000kg of the colloid substance is added into a K8000L enamel reaction kettle through a screw pump, 400L of anhydrous acetic acid and 4000L of acetone are added, the mixture is stirred for 2 hours, and a centrifuge filters 1254kg of ammonium chloride. After recovering the solvent mixture (acetic acid and acetone) from the centrifuged filtrate by reduced pressure distillation, adding 600L of water and then carrying out reduced pressure distillation, 2580kg of organic matter solution can be obtained, and the analytical data: the water content is 13.6 percent, the total nitrogen content is 9.7 percent, the chlorine content is 11.6 percent, the organic matter content is 42.3 percent, and the fluidity is good (the viscosity at 30 ℃ is 102 cP).
Example 4
At 6.25m3Per hour feed rate into the thin film evaporator Red waste stream (17.5% ammonium chloride, 51.2% moisture, 11.8% ammonium dichloroacetate, 5.6% urotropin, 1.5% glycine, 3.5% ammonium acetate, 4.3% iminodiacetic acid, 1.6% lipids, wherein lipids were presentThe substances comprise methyl methanol, acetate and methyl chloroacetate), the temperature of the film evaporator is controlled to be about 80 ℃, the vacuum degree is controlled to be-0.07 to-0.09 Mpa, and the concentrate with high viscosity (the water content is 8.1 percent, the chlorine content is 32.6 percent, the total nitrogen content is 16.3 percent, and the organic matter content is 35.6 percent) is produced.
4000kg of colloid substance is added into a K8000L enamel reaction kettle through a screw pump, 4000L of ethanol is added, and 1565kg of ammonium chloride is filtered out by a centrifuge after 2 hours of stirring. Recovering the solvent water solution from the centrifugal filtrate through reduced pressure distillation, adding 600L of water, and then performing reduced pressure distillation to obtain 2489kg of organic matter solution, wherein the analysis data is as follows: the water content is 8.6%, the total nitrogen content is 12.7%, the chlorine content is 12.6%, the organic matter content is 50.1%, and the fluidity is good (the viscosity at 30 ℃ is 120 cP).
Example 5
At 6.25m3The red waste liquid (17.5 percent of ammonium chloride, 51.2 percent of moisture, 11.8 percent of ammonium dichloroacetate, 5.6 percent of urotropine, 1.5 percent of glycine, 3.5 percent of ammonium acetate, 4.3 percent of iminodiacetic acid and 1.6 percent of lipid substances are fed into the film evaporator, wherein the lipid substances comprise methyl carbinol, acetate and methyl chloroacetate), the temperature of the film evaporator is controlled to be about 80 ℃, the vacuum degree is controlled to be-0.07 to-0.09 Mpa, and the concentrate with high viscosity (the moisture content is 8.1 percent, the chlorine content is 32.6 percent, the total nitrogen content is 16.3 percent and the organic matter content is 35.6 percent) is produced.
4000kg of colloid material is added into a K8000L enamel reaction kettle through a screw pump, 3000L of ethanol is added, after 2 hours of stirring, 1680kg of ammonium chloride is filtered out by a centrifuge (the centrifugation is slower). Recovering the solvent water solution from the centrifugal filtrate through reduced pressure distillation, adding 600L of water, and then performing reduced pressure distillation to obtain 2589kg of organic matter solution, wherein the analysis data is as follows: the water content is 12.6 percent, the total nitrogen content is 11.7 percent, the chlorine content is 7.6 percent, the organic matter content is 55.1 percent, and the fluidity is good (the viscosity at 30 ℃ is 134 cP).
Example 6
At 6.25m3Per hour feed rate into the thin film evaporator Red waste stream (17.5% ammonium chloride, 51.2% moisture, 11.8% ammonium dichloroacetate, 5.6% urotropin, 1.5% glycine, 3.5% ammonium acetate, 4.3% iminodiacetic acid, 1.6% lipids, wherein lipids were presentThe substances comprise methyl methanol, acetate and methyl chloroacetate), the temperature of the film evaporator is controlled to be about 80 ℃, the vacuum degree is controlled to be-0.07 to-0.09 Mpa, and the concentrate with high viscosity (the water content is 2.1 percent, the chlorine content is 35.6 percent, the total nitrogen content is 18.3 percent, and the organic matter content is 40.6 percent) is produced.
4000kg of the colloid is added into a K8000L enamel reaction kettle through a screw pump, 2000L of ethanol is added, after stirring for 2h, 1780kg of ammonium chloride is filtered out by a centrifugal machine (the centrifugation is slower). After recovering the solvent water solution from the centrifugal filtrate through reduced pressure distillation, adding 600L of water and then carrying out reduced pressure distillation, 2289kg of organic matter solution can be obtained, and the analysis data is as follows: 11.6 percent of water content, 15.7 percent of total nitrogen content, 8.6 percent of chlorine root content and 52.1 percent of organic matter content, and has better fluidity (the viscosity at 30 ℃ is 118 cP).
Example 7
At 6.25m3The red waste liquid (17.5 percent of ammonium chloride, 51.2 percent of moisture, 11.8 percent of ammonium dichloroacetate, 5.6 percent of urotropine, 1.5 percent of glycine, 3.5 percent of ammonium acetate, 4.3 percent of iminodiacetic acid and 1.6 percent of lipid substances are fed into the film evaporator, wherein the lipid substances comprise methyl carbinol, acetate and methyl chloroacetate), the temperature of the film evaporator is controlled to be about 80 ℃, the vacuum degree is controlled to be-0.07 to-0.09 Mpa, and the concentrate with high viscosity (the moisture content is 2.1 percent, the chlorine content is 35.6 percent, the total nitrogen content is 18.3 percent and the organic matter content is 40.6 percent) is produced.
4000kg of colloid is added into a K8000L enamel reaction kettle through a screw pump, 4000L of ethanol is added, after stirring for 2h, 2080kg of ammonium chloride is filtered out by a centrifugal machine (good centrifugation). After recovering the solvent water solution from the centrifugal filtrate through reduced pressure distillation, adding 600L of water and then carrying out reduced pressure distillation, 2689kg of organic matter solution can be obtained, and analysis data are as follows: 16.6 percent of water content, 12.7 percent of total nitrogen content, 5.6 percent of chlorine root content and 55.1 percent of organic matter content, and has better fluidity (the viscosity at 30 ℃ is 95 cP).
Claims (6)
1. A treatment device for ammonium chloride waste liquid in industrial glycine production is characterized in that a film evaporator (1) is connected with an extraction kettle (2) through a material transfer pump;
the outlet of the extraction kettle (2) is connected with a bag-pulling type centrifuge (4);
the centrifuge (4) is connected with a centrifugal filtrate tank (5), the centrifugal filtrate tank (5) is connected with a single-effect heater (6), and the single-effect heater (6) is connected with a single-effect evaporation tank (7);
the bottom of the single-effect evaporation tank (7) is connected with a secondary evaporation tank (15), and the secondary evaporation tank (15) is connected with an organic matter tank (16).
2. The device for treating the ammonium chloride waste liquid in the industrial-grade glycine production according to claim 1, wherein the top of the single-effect evaporation tank (7) is connected with the gas-phase rectifying tower (8); the top of the gas phase rectifying tower (8) is sequentially connected with a first-stage condenser (10) and a second-stage condenser (11), the second-stage condenser (11) is connected with a solvent storage tank (12), and the solvent storage tank (12) is connected with the gas phase rectifying tower (8).
3. The device for treating the ammonium chloride waste liquid in the industrial-grade glycine production according to claim 2, wherein the bottom of the gas-phase rectifying tower (8) is connected with a reboiler (9), the reboiler (9) is connected with a secondary evaporation water-replenishing tank (13), and the secondary evaporation water-replenishing tank (13) is connected with a preheater (14).
4. The device for treating the ammonium chloride waste liquid in the industrial-grade glycine production is characterized in that the preheater (14) is connected with the secondary evaporation tank (15), and the secondary evaporation tank (15) is connected with the organic matter tank (16).
5. The device for treating the ammonium chloride waste liquid in the industrial glycine production according to claim 1 or 4, wherein the top of the secondary evaporation tank (15) is connected with the secondary evaporation primary condenser (19) and the secondary evaporation secondary condenser (20) in sequence through steam pipelines and then connected with the dilute solvent tank (21).
6. The device for treating the ammonium chloride waste liquid in the industrial-grade glycine production according to claim 5, wherein a hot water tank (17) inlet pipe is further arranged at the bottom of the secondary evaporation tank (15), the hot water tank (17) is connected with a dryer (18), and the dryer (18) is connected with the hot water tank (17) to form a circulation loop; the top of the secondary evaporation tank (15) is also connected with a dryer (18) through a steam pipeline.
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