CN115215394B - Treatment process of ammonium chloride waste liquid in glycine production - Google Patents
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
The invention relates to a treatment process of ammonium chloride waste liquid in industrial grade glycine production, and mainly provides a treatment process of ammonium chloride waste liquid in glycine production from the thought of reducing chloride ion content and viscosity. The process can continuously recover the ammonium chloride product from the waste liquid, and simultaneously obtain the organic matter solution with better fluidity, wherein the ammonium chloride can be mixed with the byproduct normal ammonium chloride in glycine production for take-out, and the organic matter solution can be taken out to an organic fertilizer enterprise for mixing with the yeast solution for use in a large amount. The invention has simple process, can realize the high-value comprehensive utilization of the ammonium chloride waste liquid, has no waste water generation, can finally realize zero clearing of the red waste liquid in glycine industry, and has remarkable environmental protection benefit. Meanwhile, the recycled ammonium chloride and organic matter solution can produce economic benefits.
Description
Technical Field
The invention discloses a treatment process of ammonium chloride waste liquid in industrial grade glycine production, belongs to the technical field of chemical production, and particularly relates to a treatment method of ammonium chloride waste liquid in glycine production process by chloroacetic acid ammonolysis.
Background
Currently, the domestic industrial grade glycine production still adopts the traditional chloroacetic acid ammonolysis process, and the process can be simply described as follows: reacting chloroacetic acid aqueous solution with ammonia under the catalysis of urotropine, extracting with methanol, crystallizing, centrifuging, and drying to obtain glycine product; the centrifuged methanol mother liquor is subjected to methanol rectification, double-effect countercurrent and flash evaporation concentration, cooling crystallization, thickening and centrifugation in sequence to obtain yellow byproduct ammonium chloride which is used for producing chemical fertilizers, and a large amount of red waste liquid is produced. The process has a plurality of defects such as low yield, incapability of recovering urotropine serving as a catalyst, complex chemical reaction caused by high-temperature rectification, high-COD (chemical oxygen demand) evaporation condensate water generation, difficult treatment of red waste liquid and the like. Especially, after the national high-pressure environmental protection policy is issued in recent years, red waste liquid treatment becomes the biggest pain point of glycine enterprises.
The final red waste liquid in glycine production basically comprises: 15-20% of ammonium chloride, 40-60% of water, 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 methoxide, acetate and methyl chloroacetate. In the industry, a method of disc granulation or drum granulation is generally adopted, and the waste liquid is used for producing chloridion-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 chloridion, total nutrient, organic matters, moisture, pH and the like, the waste liquid is small in usage amount, the release of glycine productivity is affected more or less, legal utilization still cannot be completely achieved, and environmental protection risks exist.
Disclosure of Invention
The invention mainly starts from the thought of reducing the chloride ion content and viscosity of the ammonium chloride waste liquid, and provides a treatment process of the ammonium chloride waste liquid in industrial grade glycine production. According to the process, 0.2-0.4 ton of ammonium chloride product and 0.4-0.6 ton of organic matter solution can be recovered from 1 ton of waste liquid, the ammonium chloride can be mixed with normal ammonium chloride in glycine production for take-out, and the organic matter solution can be taken out to an organic fertilizer enterprise for use in a large amount after being mixed with yeast solution.
In order to achieve the purpose of the invention, the following process is adopted, and the main steps are as follows:
and (2) treating the ammonium chloride waste liquid into a concentrate with the water content of below 30%, the total nitrogen content of 9-12%, the chloride radical content of 10-15% and the organic matter content of 20%.
And (2) fully dissolving the concentrate by using a solvent, cooling to 25-30 ℃ for crystallization for 6-8h, and centrifuging to obtain ammonium chloride.
And (3) recovering the solvent by centrifugal mother decompression single-effect evaporation, and continuously adding water for decompression distillation after most of the solvent is rectified out, so that a final organic matter solution can be obtained.
Solvent vapor generated by single-effect evaporation, flash evaporation and ammonium chloride wet powder drying of the mother solution in the step (4) passes through a gas phase rectifying tower, mixed solvent meeting the application requirement can be recovered at the top of the tower, and water containing the dilute solvent at the tower bottom is returned to the system to be used as water supplementing.
The ammonium chloride waste liquid comprises 15-20% of ammonium chloride, 40-60% of water, 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 methoxide, acetate and methyl chloroacetate.
The mixed solvent comprises a mixture of at least two of methanol, ethanol, propanol, butanol, isopropanol, isobutanol, n-butanol, acetone, butanone, formic acid, methylal and acetic acid.
The method for treating the ammonium chloride waste liquid into the concentrate comprises any one of single-effect evaporation concentration, multi-effect evaporation concentration and thin film evaporation concentration.
The weight ratio of the concentrate to the mixed solvent is controlled to be 0.5-4.
The vacuum degree in the vacuum distillation process is-0.07 to-0.09 Mpa.
The invention has simple process, can realize the high-value comprehensive utilization of the ammonium chloride waste liquid, generates no waste water and economic benefit, can finally realize zero clearing of the red waste liquid in glycine industry, and has remarkable environmental protection benefit and economic benefit.
Drawings
FIG. 1 is a flow chart of a process for treating waste ammonium chloride solution in industrial grade glycine production.
Detailed Description
Example 1
500g of red waste liquid (17.5% ammonium chloride, 51.2% moisture, 11.8% ammonium dichloroacetate, 5.6% urotropine, 1.5% glycine, 3.5% ammonium acetate, 4.3% iminodiacetic acid, 1.6% lipid substances including methyl methoxide, acetate and methyl chloroacetate) were taken in a 1000ml flask and concentrated under reduced pressure of-0.07 to-0.09 Mpa to 341g of concentrate (moisture content 28.1%, chloride content 24.9%, total nitrogen content 16.3% and organic content 25.6%). 71g of methylal and 100ml of isopropanol were added, and after stirring for 2 hours, 71.3g of ammonium chloride (nitrogen content 20.8%, conversion of the purity of the ammonium chloride to 79.5%) were filtered off. Recovering solvent mixture (methylal and isopropanol) from the centrifugate through reduced pressure distillation under-0.07 to-0.09 Mpa (recovering 124.18g of solvent mixture), adding 20g of water, and then performing reduced pressure distillation under-0.07 to-0.09 Mpa to obtain 239g of organic matter solution, wherein analytical data are as follows: the water content is 19%, the total nitrogen content is 8.7%, the chloride content is 7.3%, the organic matter content is 45.7%, and the fluidity is good (absolute viscosity at 30 ℃ C. Is 55 cP).
Example 2
500g of red waste liquid (18.3% ammonium chloride, 50.4% moisture, 12.6% ammonium dichloroacetate, 6.1% urotropine, 1.7% glycine, 3.3% ammonium acetate, 4.0% iminodiacetic acid, 2.0% lipid substances including methyl methoxide, acetate and methyl chloroacetate) was concentrated under reduced pressure to 353g of concentrate (moisture content 29.5%, chloride content 25.3%, total nitrogen content 15.3% and organic matter content 24.1%) in a 1000ml flask. 71g of acetic acid and 200ml of isopropanol were added, and after stirring for 2 hours 62.3g of ammonium chloride (nitrogen content 19.8%, conversion of the purity of ammonium chloride to 75.6%) were filtered off. Recovering solvent mixture (acetic acid and isopropanol, 201.5 g) from centrifugate filtrate by vacuum distillation under-0.07 to-0.09 Mpa, adding 20g of water, and vacuum distilling under-0.07 to-0.09 Mpa to obtain 231.5g of organic solution, and analyzing data: 21.3% of moisture, 6.7% of total nitrogen, 11.2% of chloride and 47.3% of organic matters, and has good fluidity (absolute viscosity 61cP at 30 ℃).
Example 3
500g of red waste liquid (18.8% ammonium chloride, 48.7% moisture, 12.2% ammonium dichloroacetate, 6.5% urotropine, 1.8% glycine, 3.3% ammonium acetate, 4.7% iminodiacetic acid, 1.4% lipid substances including methyl methoxide, acetate, methyl chloroacetate) was concentrated under reduced pressure to 305g of concentrate (moisture content 19.6%, chloride content 26.6%, total nitrogen content 19.9%, organic content 26.4%) in a 1000ml flask under-0.07 to-0.09 Mpa. 40g of anhydrous acetic acid and 100ml of acetone were added, and after stirring for 2 hours, 54g of ammonium chloride (nitrogen content 18.5%, conversion of the purity of ammonium chloride to 70.7%) was filtered off. Recovering solvent mixture (anhydrous acetic acid and acetone, 83.3 g) from centrifugate filtrate by reduced pressure distillation under-0.07 to-0.09 Mpa, adding 20g of water, and then performing reduced pressure distillation under-0.07 to-0.09 Mpa to obtain 258g of organic matter solution, wherein analytical data are as follows: 15.6% of moisture, 8.7% of total nitrogen, 12.6% of chloride and 44.3% of organic matters, and has good fluidity (absolute viscosity 67cP at 30 ℃).
Example 4
500g of red waste liquid (18.8% ammonium chloride, 49.3% moisture, 10.7% ammonium dichloroacetate, 5.8% urotropine, 1.5% glycine, 3.4% ammonium acetate, 5.0% iminodiacetic acid, 2.4% lipid substances including methyl methoxide, acetate and methyl chloroacetate) was concentrated in a 1000ml flask under reduced pressure at-0.07 to-0.09 Mpa to 285g of concentrate (moisture content 14.2%, chloride content 32.1%, total nitrogen content 20.3% and organic matter content 28%). 200ml of butanone was added thereto, and after stirring for 2 hours, 80.2g of ammonium chloride (nitrogen content 19.1%, converted to 73% purity) was filtered off. Distilling the centrifugate under reduced pressure under-0.07 to-0.09 Mpa to recover 137g solvent butanone, adding 20g water, and distilling under reduced pressure under-0.07 to-0.09 Mpa to obtain 198g organic matter solution, and analyzing data: moisture content 18.6%, total nitrogen content 7.4%, chloride content 8.6%, organic content 62.7%, and fluidity was good (absolute viscosity 58cP at 30 ℃).
Example 5
The procedure and steps were as in example 4, 305g (moisture content 6.2%, chlorine content 27.6%, total nitrogen content 20.3%, organic content 28%) of red water concentrate was added, and only the solvent was replaced with 305ml of ethanol, 76.25g (nitrogen content 20.4%, purity 78% of ammonium chloride) of ammonium chloride was filtered, 225.3g of ethanol aqueous solution was recovered, and 242g of organic matter solution was obtained, and analysis data were obtained: 15.6% of moisture, 7.9% of total nitrogen, 6.9% of chloride, 58.9% of organic matters, and good fluidity (absolute viscosity 77cP at 30 ℃).
Example 6
The procedure and steps were as in example 4, adding 298.5g (moisture content 20.5%, chlorine content 21.6%, total nitrogen content 20.3%, organic content 24%) of red water concentrate, and only replacing the solvent with 298.5ml of propanol, filtering out 71.68g (nitrogen content 18.6%, purity of converted ammonium chloride 71%), recovering 275.3g of propanol aqueous solution, and obtaining 191.2g of organic matter solution, analysis data: 10.3% of water, 7.7% of total nitrogen, 9.6% of chloride, 68.2% of organic matters, and good fluidity (absolute viscosity 84cP at 30 ℃).
Example 7
The procedure and steps were as in example 4, except that 300g of red water concentrate (moisture content 4.5%, chlorine radical content 23.6%, total nitrogen content 21.4%, organic matter content 26.4%) was added and only the solvent was replaced with 300ml of methanol, 84.3g of ammonium chloride (nitrogen content 21.1%, purity of the converted ammonium chloride 80.6%) was filtered, 308.5g of aqueous methanol solution was recovered, 147.2g of organic matter solution was obtained, and analysis data were obtained: the water content is 7.6%, the total nitrogen content is 10.2%, the chloride content is 10.6%, the organic matter content is 65.9%, and the fluidity is good (absolute viscosity 95cP at 30 ℃).
Example 8
The procedure and procedure were as in example 4, 302g (moisture content 18.6%, chlorine content 21.6%, total nitrogen content 20.8%, organic content 27.4%) of red water concentrate was added, and only the solvent was replaced with a mixture of methanol and formic acid, wherein 280ml of methanol and 22ml of formic acid were used, 90.6g (nitrogen content 20.1%, purity of converted ammonium chloride 76.8%) of ammonium chloride was filtered out, 279.6g of solvent aqueous solution was recovered to obtain 200.24g of organic solution, and analysis data were obtained: 17.6% of moisture, 7.2% of total nitrogen, 6.6% of chloride and 61.3% of organic matters, and has good fluidity (absolute viscosity 57cP at 30 ℃).
Example 9
The procedure and steps were as in example 4, 303g (moisture content 18.6%, chlorine content 21.6%, total nitrogen content 20.8%, organic content 27.4%) of red water concentrate was added, and only the solvent was replaced with a mixture of methanol and acetic acid, wherein 280ml of methanol and 22ml of acetic acid were used to filter out 84.2g of ammonium chloride (nitrogen content 18.1%, purity of converted ammonium chloride 69.2%), 291.5g of aqueous solvent was recovered to obtain 173.9g of organic solution, and analysis data were obtained: 11.6% of water, 5.2% of total nitrogen, 7.6% of chloride, 65.4% of organic matters, and good fluidity (absolute viscosity 63cP at 30 ℃).
Example 10
The procedure and steps were as in example 4, except that 303g (moisture content: 18.6%, chlorine radical content: 21.6%, total nitrogen content: 20.8%, organic content: 27.4%) of red water concentrate was added and only the solvent was replaced with 303ml of methylene chloride, 100.2g (nitrogen content: 14.1%, purity of the converted ammonium chloride: 53.9%) of ammonium chloride was filtered, 289g of aqueous solvent solution was recovered, and 315.3g of organic matter solution was obtained, and data were analyzed: 17.6% of moisture, 4.2% of total nitrogen, 9.6% of chloride, 59.3% of organic matters, and good fluidity (absolute viscosity 59cP at 30 ℃).
Example 11
The procedure and steps were as in example 4, except that 301g (moisture content: 18.6%, chlorine radical content: 21.6%, total nitrogen content: 20.8%, organic matter content: 27.4%) of red water concentrate was added and only that the solvent was replaced with 301ml of methylal, 89.2g (nitrogen content: 19.1%, purity of converted ammonium chloride: 72.9%) of ammonium chloride was filtered, 270g of aqueous solvent solution was recovered, and 200.9g of organic matter solution was obtained, and data were analyzed: 27.6% of moisture, 4.7% of total nitrogen, 5.6% of chloride and 55.3% of organic matters, and has good fluidity (absolute viscosity 61cP at 30 ℃).
Example 12
The method and procedure were as in example 4, 298g (moisture content 18.6%, chlorine radical content 21.6%, total nitrogen content 20.8%, organic content 27.4%) of red water concentrate was added, and only the solvent was replaced with N, N-dimethylformamide, the dissolution process could not be completed, and ammonium chloride could not be obtained by filtration, and an organic solution with good fluidity could not be obtained.
Claims (3)
1. The treatment process of ammonium chloride waste liquid in glycine production is characterized in that after the ammonium chloride waste liquid is added into a mixed solvent for dissolution, cooling crystallization and centrifugation are carried out to obtain ammonium chloride, wherein the ammonium chloride waste liquid comprises 15-20% of ammonium chloride, 40-60% of water, 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 methoxide, acetate and methyl chloroacetate, the ammonium chloride waste liquid is concentrated until the water content is below 30% before being added into the mixed solvent for dissolution, and the method for treating the ammonium chloride waste liquid into a concentrate comprises any one of single-effect evaporation concentration, multi-effect evaporation concentration and film evaporation concentration;
the mother solution after centrifugation is subjected to reduced pressure distillation to recover a mixed solvent, the rest of the mixture is continuously added with water, and an organic matter solution is obtained through reduced pressure distillation, wherein the mixed solvent comprises one or a mixture of a plurality of methanol, ethanol, propanol, butanol, isopropanol, isobutanol, n-butanol, acetone, butanone, formic acid, methylal, acetic acid, dichloromethane, chloroform and carbon tetrachloride.
2. The process for treating waste ammonium chloride solution in glycine production according to claim 1, wherein the weight ratio of the concentrate to the mixed solvent is controlled to be 0.5-4.
3. The process for treating an ammonium chloride waste liquid in glycine production according to claim 1, wherein the vacuum degree in the reduced pressure distillation process is-0.07 to-0.09 Mpa.
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| DE3061083D1 (en) * | 1979-02-15 | 1982-12-23 | Bayer Antwerpen Nv | Process for working up waste water containing ammonium sulfate |
| JPH0692917A (en) * | 1992-07-16 | 1994-04-05 | Hakko Tsusho Kk | Improved method of synthesizing glycine |
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