CN109650646B - Treatment method of glycine production wastewater - Google Patents

Treatment method of glycine production wastewater Download PDF

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CN109650646B
CN109650646B CN201811392169.0A CN201811392169A CN109650646B CN 109650646 B CN109650646 B CN 109650646B CN 201811392169 A CN201811392169 A CN 201811392169A CN 109650646 B CN109650646 B CN 109650646B
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mother liquor
glycine
heating
liquid
activated sludge
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CN109650646A (en
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卢淑婷
宋铁犇
王秀茹
宋秋月
王立辉
蔡建红
曹甲宁
韩素娟
朱晓伦
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HEBEI DONGHUA JIHENG CHEMICAL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/38Treatment of water, waste water, or sewage by centrifugal separation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/16Nitrogen compounds, e.g. ammonia
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/34Organic compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/36Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00Biological treatment of water, waste water, or sewage
    • C02F3/02Aerobic processes
    • C02F3/12Activated sludge processes

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  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Removal Of Specific Substances (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)

Abstract

The invention discloses a treatment method of glycine production wastewater, belonging to the technical field of wastewater treatment, wherein the production method of glycine is a chloroacetic acid ammoniation method, methanol is firstly distilled out from ammoniated mother liquor after glycine is produced, and then rectified mother liquor obtained after methanol is distilled out is treated, and the treatment steps are as follows: 1) heating the rectification mother liquor to boil, allowing steam to pass through a slightly boiling sulfuric acid solution, and collecting effluent liquid to obtain a collection liquid; 2) adding slaked lime into the collected liquid, adjusting the pH value to 11-12, heating until the color of the reaction system is changed from colorless to faint yellow, and then cooling to obtain secondary collected liquid; 3) and adjusting the pH value of the secondary collection liquid to 6.5-7, then dropwise adding the secondary collection liquid into the activated sludge solution while carrying out aeration, and continuing aeration after dropwise adding is finished. The wastewater treated by the method meets the pollution discharge standard, and can be used for absorbing hydrochloric acid tail gas in a hydrochloric acid working section, so that the effective utilization of resources is realized; and the process flow is simple and the investment cost is low.

Description

Treatment method of glycine production wastewater
Technical Field
The invention relates to the technical field of glycine wastewater treatment and environmental protection, in particular to a comprehensive treatment technology for glycine production wastewater.
Background
The content and concentration of pollutants in the glycine production wastewater are high, a large amount of ammonia is needed to be used as a raw material in the glycine production process, the formed wastewater is large in amount, the ammonia nitrogen value is very high, the treatment difficulty is very high, and the wastewater produced in the chloroacetic acid ammonification method production process contains up to 20% of ammonium chloride, and also contains glycine and urotropine with the total amount exceeding 10%, and also contains a large amount of methanol and formaldehyde. The existing treatment process is that after glycine is separated, an evaporation process is adopted for ammoniation mother liquor, methanol in the ammoniation mother liquor is evaporated, collected and recycled, then a great amount of double-effect water is evaporated from rectification mother liquor by a double-effect evaporation process, then the temperature is reduced to crystallize and separate out ammonium chloride in filter residues, the obtained ammonium chloride solid can be sold as a chemical fertilizer, but a great amount of evaporated double-effect water contains more pollutants such as urotropine, ammonia nitrogen waste, formaldehyde and the like and higher COD; at present, the treatment process aiming at the double-effect water mostly utilizes a membrane separation technology to recover urotropine in the double-effect water for recycling, but the method has higher manufacturing cost of the membrane, shorter service life of the membrane and higher operation cost, and the treated waste liquid has more pollutant types and contents and is difficult to discharge to reach the standard, thereby becoming the difficult problem in the aspect of environmental protection of the industry.
Wanfang et al treated the wastewater after triple effect evaporation, and reduced organic compounds such as ammonia nitrogen and formaldehyde by a blow-off method and a Fenton method, the blow-off method was suitable for the treatment of high concentration formaldehyde and ammonia nitrogen, and although the Fenton method could reduce formaldehyde and COD, the treated solution was difficult to reach the discharge standard due to the yellow color of ferric iron, and the blow-off method and the Fenton method had higher operating costs.
So far, no complete and low-cost treatment standard-reaching process acceptable by enterprises exists for treating the double-effect water generated in the glycine industry, and the economic and applicable wastewater treatment technology is urgently found along with the increase of the environmental protection pressure of the enterprises.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a treatment method of glycine production wastewater, which realizes the cyclic utilization of glycine production wastewater and reduces the environmental pollution.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a glycine production wastewater treatment method, wherein the glycine production method is a chloroacetic acid ammoniation method, ammoniated mother liquor after glycine production is firstly heated and evaporated to remove methanol in the ammoniated mother liquor, the methanol is recycled in a workshop, and then rectified mother liquor after the methanol evaporation is treated, and the treatment steps are as follows:
1) heating the rectification mother liquor to boil, allowing steam to pass through a slightly boiling sulfuric acid solution, and collecting effluent liquid to obtain a collection liquid; centrifuging residues left by evaporation of the rectification mother liquor to obtain ammonium chloride;
2) adding slaked lime into the collected liquid, adjusting the pH value to 11-12, heating until the color of the reaction system is changed from colorless to faint yellow, and then cooling to obtain a secondary collected liquid;
3) and adjusting the pH value of the secondary collection liquid to 6.5-7, then dropwise adding the secondary collection liquid into the activated sludge solution, carrying out aeration while dropwise adding, and continuing aeration for 3-8 hours after dropwise adding is finished.
The technical scheme of the invention is further improved as follows: the step 1) of heating the rectification mother liquor to boiling comprises the steps of firstly adding a proper amount of rectification mother liquor into a reaction container, heating to boiling, and then dropwise adding supplementary rectification mother liquor into the reaction container while heating.
The technical scheme of the invention is further improved as follows: the concentration of the sulfuric acid solution used in the step 1) is 20-30%.
The technical scheme of the invention is further improved as follows: the slightly boiling sulfuric acid solution is prepared by heating the sulfuric acid solution to 110-120 ℃.
The technical scheme of the invention is further improved as follows: the adding amount of the slaked lime in the step 2) is that 0.3-1.6 g of slaked lime is added into each liter of the collecting liquid.
The technical scheme of the invention is further improved as follows: in the step 2), heating is carried out in a water bath at 50-80 ℃ for 0.5-2 h, and cooling is carried out until the temperature is reduced to room temperature.
The technical scheme of the invention is further improved as follows: the volume ratio of the secondary collection liquid to the activated sludge solution in the step 3) is 1: 6-8.
The technical scheme of the invention is further improved as follows: the sedimentation ratio of the activated sludge solution in the step 3) is 20-60%.
The technical scheme of the invention is further improved as follows: the activated sludge solution in the step 3) is obtained by adopting, domesticating and culturing in a domestic sewage domestication pond. The domestic sewage is preferably domestic sewage of the company, the domestic sewage of the company has the advantage of easy domestication, and the domestic sewage produced by the company can be utilized.
The technical scheme of the invention is further improved as follows: the acclimatization and culture process of the activated sludge solution comprises the steps of firstly adding a proper amount of flour, then aerating for 12 hours, and then repeating the operations of adding the flour twice and then aerating for 12 hours.
Due to the adoption of the technical scheme, the invention has the technical progress that:
the wastewater treated by the method can meet the pollution discharge standard and realize resource recycling; and the process flow is simple, the investment cost is low, three wastes are not generated, and the method is convenient for industrial large-scale wastewater treatment.
The treatment method of the invention can almost completely remove urotropine in the rectification mother liquor, the removal rate of formaldehyde and ammonia nitrogen can reach more than 99%, the removal rate of COD can also reach more than 85%, the pollutant removal effect is obvious, and the treated wastewater can reach the pollution discharge standard and can be directly discharged; can also be pumped back to the hydrochloric acid workshop section for recycling, thereby realizing the recycling of resources.
The process method is simple, only needs to heat and boil the rectification mother liquor, add slaked lime after the rectification mother liquor passes through a sulfuric acid solution, and finally add the slaked lime into an activated sludge solution for treatment, and the steps are simple; and expensive equipment investment and reagents are not needed, the treatment cost is low, the method is suitable for industrial large-scale wastewater treatment, and the practical application value is high.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples:
example 1
A glycine production wastewater treatment method, wherein the glycine production method is a chloroacetic acid ammoniation method, after glycine is produced, the residual wastewater (ammoniated mother liquor) is firstly heated and evaporated to remove methanol in the glycine, the methanol is pumped back to a workshop for recycling, then the rectified mother liquor after the methanol evaporation is treated, and the treatment steps of the rectified mother liquor are as follows:
1) heating the rectification mother liquor in a reaction container to boil, introducing a slightly boiling (heating temperature of 110 ℃) sulfuric acid solution with the concentration of 20% into steam of the rectification mother liquor through a conduit, collecting effluent liquid passing through sulfuric acid to obtain a collection liquid, and centrifuging residues left after the rectification mother liquor is evaporated to obtain ammonium chloride. The process of heating the rectification mother liquor to boiling comprises the steps of firstly adding a proper amount of rectification mother liquor into a reaction container, then heating to boiling, and then dropwise adding the rectification mother liquor into the reaction container while heating to supplement the consumption of the rectification mother liquor.
2) And adding slaked lime into the collected liquid, wherein the adding amount of the slaked lime is 1.6g of slaked lime added into each liter of the collected liquid, adjusting the pH value to 11 by using NaOH, carrying out water bath at the temperature of 70 ℃ for 0.5-2 h until the color of the system changes from colorless to slightly yellow, stopping, and cooling to room temperature to obtain a secondary collected liquid.
3) And adjusting the pH value of the secondary collection liquid to 6.5 by using hydrochloric acid, then dropwise adding the secondary collection liquid into the activated sludge solution while carrying out aeration, and continuously aerating for 3-8 hours after dropwise adding is finished. The activated sludge solution is obtained by domesticating and culturing domestic sewage of the company, and the specific domestication and culture process comprises the steps of adding a proper amount of flour, aerating for 12 hours, then repeating the operations of adding flour twice and aerating for 12 hours, wherein the sedimentation ratio of the prepared activated sludge solution is 20-60%; the volume ratio of the secondary collection liquid to the activated sludge solution is 1: 6.
Example 2
A glycine production wastewater treatment method, wherein the glycine production method is a chloroacetic acid ammoniation method, after glycine is produced, the residual wastewater (ammoniated mother liquor) is firstly heated and evaporated to remove methanol in the glycine, the methanol is pumped back to a workshop for recycling, then the rectified mother liquor after the methanol evaporation is treated, and the treatment steps of the rectified mother liquor are as follows:
1) heating the rectification mother liquor in a reaction container to boil, introducing the steam into a slightly boiling (heating temperature is 120 ℃) sulfuric acid solution with the concentration of 30% through a conduit, collecting the effluent liquid passing through the sulfuric acid to obtain a collection liquid, and centrifuging the residue left by evaporation of the rectification mother liquor to obtain the ammonium chloride. Wherein, the process of heating the rectification mother liquor to boiling comprises the steps of firstly adding a small amount of rectification mother liquor into a reaction vessel, then heating to boiling, and then dropwise adding the rectification mother liquor into the reaction vessel while heating to supplement the consumption of the mother liquor.
2) And adding slaked lime into the collected liquid, wherein the adding amount of the slaked lime is that 0.3g of slaked lime is added into each liter of the collected liquid, adjusting the pH value to 12 by using NaOH, carrying out water bath at the temperature of 80 ℃ for 0.5-2 h until the color of the system changes from colorless to slightly yellow, stopping, and cooling to room temperature to obtain secondary collected liquid.
3) And (3) regulating the pH value of the secondary collection liquid to 7 by using hydrochloric acid, then dropwise adding the secondary collection liquid into the activated sludge solution while carrying out aeration, and continuing aeration for 3-8 hours after dropwise adding is finished. The activated sludge solution is obtained by domesticating and culturing domestic sewage, and the specific domestication and culture process comprises the steps of adding a proper amount of flour, aerating for 12 hours, repeating the operations of adding flour twice and aerating for 12 hours, wherein the sedimentation ratio of the prepared activated sludge solution is 20-60%; the volume ratio of the secondary collection liquid to the activated sludge solution is 1: 8.
Example 3
A glycine production wastewater treatment method, wherein the glycine production method is a chloroacetic acid ammoniation method, after glycine is produced, the residual wastewater (ammoniated mother liquor) is firstly heated and evaporated to remove methanol in the glycine, the methanol is pumped back to a workshop for recycling, then the rectified mother liquor after the methanol evaporation is treated, and the treatment steps of the rectified mother liquor are as follows:
1) heating the rectification mother liquor in a reaction container to boil, introducing the steam into a slightly boiling (heating temperature is 115 ℃) sulfuric acid solution with the concentration of 25% through a conduit, collecting the effluent liquid passing through the sulfuric acid to obtain a collection liquid, and centrifuging the residue left by evaporation of the rectification mother liquor to obtain the ammonium chloride. Wherein, the process of heating the rectification mother liquor to boiling comprises the steps of firstly adding a small amount of rectification mother liquor into a reaction vessel, then heating to boiling, and then dropwise adding the rectification mother liquor into the reaction vessel while heating to supplement the consumption of the mother liquor.
2) And adding slaked lime into the collected liquid, wherein the adding amount of the slaked lime is that 0.9g of slaked lime is added into each liter of the collected liquid, adjusting the pH value to 11.5 by using NaOH, carrying out water bath at the temperature of 50 ℃ for 0.5-2 h until the color of the system is changed from colorless to slightly yellow, and then cooling to the room temperature to obtain a secondary collected liquid.
3) And adjusting the pH value of the secondary collection liquid to 6.8 by using hydrochloric acid, then dropwise adding the secondary collection liquid into the activated sludge solution while carrying out aeration, and continuously aerating for 3-8 hours after dropwise adding is finished. The activated sludge solution is obtained by domesticating and culturing domestic sewage of the company, and the specific domestication and culture process comprises the steps of adding a proper amount of flour, aerating for 12 hours, then repeating the operations of adding flour twice and aerating for 12 hours, wherein the sedimentation ratio of the prepared activated sludge solution is 20-60%; the volume ratio of the secondary collection liquid to the activated sludge solution is 1: 7.
Comparative examples 1 to 4
Comparative examples 1 to 4 are comparative tests of example 1, with the difference that comparative example 1 exchanges the order of step 1) and step 2) in example 1; comparative example 2 the treatment operation of step 3) in example 1 is carried out first, and then the operations of steps 1) and 2) are carried out in sequence; comparative example 3 the treatment operation of step 2) in example 1 was performed first, and then the treatment operations of steps 3) and 1) were performed in sequence; comparative example 4 the treatment operation of step 3) in example 1 was carried out first, and then the treatment operations of steps 2) and 1) were carried out in this order, with the remaining parameters being the same as in example 1.
Comparative example 5
Comparative example 5 is a comparative test to example 2, with the difference that the acid used in step 1) of comparative example 5 is hydrochloric acid, and the remaining parameters are the same as in example 2.
Comparative examples 6 to 7
Comparative examples 6 to 7 are comparative tests to example 3, with the difference that comparative example 6, in step 2), slaked lime is added in an amount of 0.15g of slaked lime per litre of collected liquor; comparative example 7 the amount of slaked lime added in step 2) was 2.5g of slaked lime per liter of the collected liquid, and the remaining parameters were the same as in example 3.
Comparative examples 8 to 9
Comparative examples 8 to 9 are comparative tests of example 3, except that the volume ratio of the secondary collected liquid to the activated sludge solution in step 3) of comparative example 8 was 1:3, and the volume ratio of the secondary collected liquid to the activated sludge solution in step 3) of comparative example 9 was 1:9, and the remaining parameters were the same as in example 3.
In order to illustrate the advantages of the invention, indexes of various pollutants before and after the treatment of the double-effect water of the examples 1-3 and the comparative examples 1-9 are detected, and the detection results are shown in the following table:
TABLE 1
Figure BDA0001874321240000071
As can be seen from Table 1, the pollution discharge standard can be met only by adopting the defined reagents and parameters according to the operation steps of the invention and simultaneously removing or reducing urotropine, formaldehyde, ammonia nitrogen and COD in the rectification mother liquor to the maximum extent.

Claims (6)

1. A glycine waste water processing method, wherein the production method of glycine is a chloroacetic acid ammonification method, the ammonification mother liquor after producing glycine firstly distills methanol in the ammonification mother liquor to obtain rectification mother liquor, characterized in that: the treatment steps of the rectification mother liquor are as follows:
1) heating the rectification mother liquor to boiling, allowing steam to pass through a slightly boiling sulfuric acid solution, collecting effluent liquid to obtain a collection liquid, wherein the concentration of the sulfuric acid solution is 20-30%, and the slightly boiling sulfuric acid solution is obtained by heating the sulfuric acid solution to 110-120 ℃;
2) adding 0.3-1.6 g of slaked lime into each liter of collected liquid, adjusting the pH value to 11-12 by using sodium hydroxide, heating until the color of a reaction system is changed from colorless to faint yellow, and then cooling to obtain secondary collected liquid;
3) and adjusting the pH value of the secondary collection liquid to 6.5-7, then dropwise adding the secondary collection liquid into the activated sludge solution, wherein the volume ratio of the secondary collection liquid to the activated sludge solution is 1: 6-8, carrying out aeration while dropwise adding, and continuing aeration for 3-8 hours after dropwise adding.
2. The method for treating wastewater from glycine production as claimed in claim 1, wherein: the step 1) of heating the rectification mother liquor to boiling comprises the steps of firstly adding a proper amount of rectification mother liquor into a reaction container, heating to boiling, and then dropwise adding supplementary rectification mother liquor into the reaction container while heating.
3. The method for treating wastewater from glycine production as claimed in claim 1, wherein: in the step 2), heating is carried out in a water bath at 50-80 ℃ for 0.5-2 h, and cooling is carried out until the temperature is reduced to room temperature.
4. The method for treating wastewater from glycine production as claimed in claim 1, wherein: the sedimentation ratio of the activated sludge solution in the step 3) is 20-60%.
5. The method for treating wastewater from glycine production as claimed in claim 1, wherein: the activated sludge solution in the step 3) is obtained by adopting, domesticating and culturing in a domestic sewage domestication pond.
6. The method for treating wastewater from glycine production as claimed in claim 5, wherein: the acclimatization and culture process of the activated sludge solution comprises the steps of firstly adding a proper amount of flour, then aerating for 12 hours, and then repeating the operations of adding the flour twice and then aerating for 12 hours.
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