CN104445278A - Process for recycling clean waste liquid of polyvinyl chloride produced by calcium carbide method to caustic soda primary brine - Google Patents
Process for recycling clean waste liquid of polyvinyl chloride produced by calcium carbide method to caustic soda primary brine Download PDFInfo
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- CN104445278A CN104445278A CN201410621880.4A CN201410621880A CN104445278A CN 104445278 A CN104445278 A CN 104445278A CN 201410621880 A CN201410621880 A CN 201410621880A CN 104445278 A CN104445278 A CN 104445278A
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- caustic soda
- primary brine
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Removal Of Specific Substances (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention belongs to the technical field of chlor-alkali chemical industry, and discloses a process for recycling clean waste liquid of polyvinyl chloride produced by a calcium carbide method to caustic soda primary brine. The process comprises the following steps of: (1) removing acetylene gas contained in the clean waste liquid; (2) adding sodium hypochlorite to control available chlorine content to 0.06%-0.10%, adding hydrochloric acid to regulate a pH value to 2-5, and reacting for 10-30 minutes; (3) adding sodium hydroxide to regulate the pH value to be more than 12, reacting for 30-60 minutes, filtering, and depositing; (4) mixing filter liquor and the caustic soda primary brine, increasing temperature to 55-65 DEG C, adding sodium chloride, and controlling the content of sodium chloride to be more than 300 g/L; (5) adding sodium hydroxide to control the pH value to 10-12, adding ferric chloride hexahydrate, and reacting for more than 60 minutes, wherein the addition amount of ferric chloride hexahydrate is 0.08-0.12 g/L; (6) adding sodium carbonate, and reacting for more than 60 minutes, wherein the dose of sodium carbonate is controlled to be 0.3-0.8 g/L; (7) filtering, wherein the filter liquor is an intermediate product which reaches the effluent standard of primary brine. The process disclosed by the invention can be used for reducing the discharge of the waste liquid, preventing the high chloride content from causing that total effluent water can not reach the standard, reducing the content of calcium, magnesium and silicon, recycling a primary brine section and reducing the usage amount of brine.
Description
Technical field
The invention belongs to chemical industry for making chlorine and alkali technical field, be specifically related to the technique of the peace and quiet thin stillage recycling of a kind of generated by polyvinyl chloride by calcium carbide to caustic soda primary brine.
Background technology
China's energy structure feature is many coals, oil-poor, weak breath, and therefore domestic PVC (PVC) resin manufacturing processes route is based on carbide acetylene method.Within 2013, PVC production capacity reaches 2,476 ten thousand tons/year, and wherein calcium carbide process PVC production capacity accounts for 82% of aggregated capacity.In carbide acetylene method production process, need in the peace and quiet process of thick acetylene gas with containing effective chlorine content in 0.08 ~ 0.12% scope, pH value be 7-8 chlorine bleach liquor the impurity oxygen such as S, P are changed into acidic substance, again with rare caustic soda soln removing acidic substance, in this process, create a large amount of useless chlorine bleach liquores.
For 200,000 tons/year of PVC production equipments, under normal production scenarios, per hourly about 45m need be used
3chlorine bleach liquor, useless chlorine bleach liquor after the peace and quiet tower of two-stage is peace and quiet contains higher muriate, average chloride ion content is at 1500 more than mg/L, also containing calcium ions and magnesium ions, vitriol, phosphoric acid salt etc., a large amount of acetylene gas is dissolved with in addition in useless chlorine bleach liquor, COD content is also up to 400 ~ 600mg/L, and the usual way of industry is outer row.Henan Province implements " salt industry, alkali industry chloride emission standard " on May 1st, 2012, and in clear stipulaties waste water, chloride emission concentration is less than 350mg/L.If this part waste water is arranged outward, total draining chlorion can be caused to exceed standard, environment protection emission requirement can not be met, and water resources does not fully utilize.
Summary of the invention
The object of the invention is the technique providing the peace and quiet thin stillage recycling of a kind of generated by polyvinyl chloride by calcium carbide to caustic soda primary brine.
For achieving the above object, the present invention adopts following technical scheme:
The peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, comprises the steps:
1) (vacuum analysis and aerating apparatus is utilized) and removes the acetylene gas in peace and quiet waste liquid;
2) adding clorox control available chlorine content is 0.06-0.10%, and adding salt acid for adjusting pH value is 2-5, reaction 10-30min;
3) more than sodium hydroxide adjust ph to 12 is added, reaction 30-60min, filtering-depositing;
4) filtrate mixes with caustic soda primary brine, is warming up to 55-65 DEG C, adds sodium-chlor, controls sodium chloride content and is greater than 300g/L; Wherein, described filtrate and the blending ratio of caustic soda primary brine equal the ratio of peace and quiet waste liquid total Water and primary brine total Water;
5) adding sodium hydroxide control ph is 10-12, adds ferric chloride (FeCl36H2O), and the add-on of ferric chloride (FeCl36H2O) is 0.08-0.12g/L, reaction more than 60min;
6) add sodium carbonate, control sodium carbonate relative to the excessive 0.3-0.8g/L of calcium ion, reaction more than 60min;
7) filter, filtrate being reaches the middle product of primary brine Effluent criteria, and wherein calcium magnesium total content is less than 4 PPm, and silicone content is less than 2.3PPm.
Further, in step 1), described peace and quiet waste liquid is the useless chlorine bleach liquor that generated by polyvinyl chloride by calcium carbide acetylene cleaning workshop section produces.
Preferably, in step 1), in the peace and quiet waste liquid after removing acetylene gas, COD is 100-150mg/L.
Preferably, step 2) in, described clorox adds with its solution form, and is selected from the chlorine bleach liquor of caustic soda synthesizing section tail chlorine absorption tower generation; Step 2) in, described hydrochloric acid is selected from the hydrochloric acid of production of caustic soda hydrogen chloride synthesis workshop section; Step 3) and 5) in, described sodium hydroxide adds with its solution form, and is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section; In step 4), described primary brine is selected from the primary brine of production of caustic soda primary brine workshop section, chloride content 90-110g/L; In step 4), described sodium-chlor is selected from production of caustic soda raw material solid sodium-chlor; In step 5), described ferric chloride (FeCl36H2O) adds with its solution form, and is selected from the ferric chloride (FeCl36H2O) of production of caustic soda primary brine workshop section use; In step 6), described sodium carbonate adds with its solution form, and is selected from the sodium carbonate solution of production of caustic soda primary brine workshop section.
The principal reaction that the method for the invention relates to has:
PO
3 3-+ClO
-=PO
4 3-+Cl
-
3Ca
2++2PO
4 3- =Ca
3(PO
4)
2↓
3Mg
2++2PO
4 3-=Mg
3(PO
4)
2↓
Mg
2++2OH
- =Mg(OH)
2↓
Fe
3++3OH
- =Fe(OH)
3↓
Ca
2++CO
3 2- =CaCO
3↓
Ca
2+ +SiO
3 2- =CaSiO
3↓
Compared to the prior art, present invention process has the following advantages:
1. clorox waste liquid obtains effective utilization, is mixed with caustic soda primary brine the middle product meeting index request after primary refined brine, can economized salt water consumption;
2. decrease the outer discharge capacity of waste liquid and processing costs, can avoid causing Zong Xiashui not up to standard because chloride content exceeds standard;
3. effectively reduce calcium magnesium silicon ion content in solution, meet productive capacity requirement;
4. do not increase external source, do not introduce foreign ion, desired raw material is raw material and the intermediates of Production of PVC and production of caustic soda use.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Now the present invention is further illustrated in conjunction with the accompanying drawings and embodiments, but protection scope of the present invention is not limited thereto.
In the actual production line of annual output 200000 tons of polyvinyl chloride (PVC) RESINS that applicant is current and annual output 200000 tons of ion film caustic sodas, the generation total amount of the peace and quiet waste liquid of generated by polyvinyl chloride by calcium carbide acetylene cleaning workshop section is 45m3/h, and the generation total amount of production of caustic soda primary brine is 240m3/h.Generated by polyvinyl chloride by calcium carbide acetylene cleaning workshop section needs to prepare chlorine bleach liquor, during preparation, peace and quiet waste liquid can be adopted to replace part water, prepare the ratio that peace and quiet waste liquid amount used accounts for peace and quiet waste liquid total amount and be compound proportion, after composite, the peace and quiet waste liquid stayed is the peace and quiet waste liquid treating reuse.
embodiment 1
As shown in Figure 1, the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide is to the technique of caustic soda primary brine, and it comprises the steps:
1) in 20L double-layer glass reaction kettle, add 5L to place for some time and be taken to generated by polyvinyl chloride by calcium carbide acetylene cleaning workshop section and do not carry out composite but through the peace and quiet waste liquid (in the peace and quiet waste liquid after process, COD is 125mg/L) of Air Exposure, wherein available chlorine content is almost nil after testing; Add 50mL chlorine bleach liquor, wherein available chlorine content is 0.1% after testing, with salt acid for adjusting pH to 2, and reaction 10min, then regulate pH to 12 with sodium hydroxide solution, reaction 30min, filtering-depositing; Described chlorine bleach liquor is selected from the secondary sodium that caustic soda synthesizing section tail chlorine absorption tower produces, and the available chlorine content in secondary sodium is 118g/L; Described hydrochloric acid is selected from the hydrochloric acid of production of caustic soda hydrogen chloride synthesis workshop section, and mass percent concentration is 30%; Described sodium hydroxide solution is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section, and mass percent concentration is 32%.
2) get filtrate 1L and rejoin 20L double-layer glass reaction kettle, mix with 5L primary brine, fully stir, be warming up to 55 DEG C, add 1150g solid sodium chloride, be stirred to sodium-chlor and dissolve completely; Described primary brine is selected from the primary brine of production of caustic soda primary brine workshop section, chloride content 90g/L; Described sodium-chlor is selected from production of caustic soda primary brine workshop section raw material solid sodium-chlor, and the mass percentage of sodium-chlor is greater than 94%.
3) add sodium hydroxide solution and regulate pH to 11, add the solution with the preparation of 0.5g ferric chloride (FeCl36H2O), reaction 60min; Detection calcium ion content is 223mg/L, adds 62mL sodium carbonate solution, reaction 60min, and precipitate with triumphant membrane filtration, filtrate being reaches the middle product of primary brine Effluent criteria; Described sodium hydroxide solution is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section, and mass percent concentration is 32%; Described ferric chloride (FeCl36H2O) is selected from the ferric chloride (FeCl36H2O) that production of caustic soda primary brine workshop section uses; Described sodium carbonate solution is selected from the sodium carbonate solution of production of caustic soda primary brine workshop section, content 100g/L; Described triumphant film is selected from the HVM film of production of caustic soda primary brine workshop section.
After measured, reach in the middle product of primary brine Effluent criteria: calcium contents 850ppb, Mg content 20ppb, silicone content 1.70ppm.Wherein available chlorine content adopts iodimetry,iodometry, carries out with reference to the measuring method of available chlorine content in " GB 19106-2003 chlorine bleach liquor "; The silica test of calcium magnesium selects the U.S.'s graceful ICP plasma emission spectrometer of profit to carry out, lower same.
embodiment 2
As shown in Figure 1, generated by polyvinyl chloride by calcium carbide peace and quiet thin stillage recycling caustic soda primary brine technique, it comprises the steps:
1) in 20L double-layer glass reaction kettle, add 5L and be taken to generated by polyvinyl chloride by calcium carbide acetylene cleaning workshop section compound proportion 50% and through the peace and quiet waste liquid (in the peace and quiet waste liquid after process, COD is 117mg/L) of Air Exposure, wherein available chlorine content is 0.03% after testing; Add 25mL chlorine bleach liquor, wherein available chlorine content is 0.08% after testing, with salt acid for adjusting pH to 3, and reaction 20min, then regulate pH to 12 with sodium hydroxide solution, reaction 45min, filtering-depositing; Described chlorine bleach liquor is selected from the secondary sodium that caustic soda synthesizing section tail chlorine absorption tower produces, and the available chlorine content in secondary sodium is 118g/L; Described hydrochloric acid is selected from the hydrochloric acid of production of caustic soda hydrogen chloride synthesis workshop section, and concentration is 30%; Described sodium hydroxide solution is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section, and mass percent concentration is 32%.
2) get filtrate 1L and rejoin 20L double-layer glass reaction kettle, mix with 10L primary brine, fully stir, be warming up to 60 DEG C, add 1825g solid sodium chloride, be stirred to sodium-chlor and dissolve completely; Described primary brine is selected from the primary brine of production of caustic soda primary brine workshop section, chloride content 100g/L; Described sodium-chlor is selected from production of caustic soda primary brine workshop section raw material solid sodium-chlor, and sodium chloride content is greater than 94%.
3) add sodium hydroxide solution and regulate pH to 11, add the solution with the preparation of 1g ferric chloride (FeCl36H2O), reaction 60min; Detection calcium ion content is 178mg/L, adds 110mL sodium carbonate solution, reaction 60min, and precipitate with triumphant membrane filtration, filtrate being reaches the middle product of primary brine Effluent criteria; ; Described sodium hydroxide solution is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section, and mass percent concentration is 32%; Described ferric chloride (FeCl36H2O) is selected from the ferric chloride (FeCl36H2O) that production of caustic soda primary brine workshop section uses; Described sodium carbonate solution is selected from the sodium carbonate solution of production of caustic soda primary brine workshop section, content 100g/L; Described triumphant film is selected from the HVM film of production of caustic soda primary brine workshop section.
After measured, reach in the middle product of primary brine Effluent criteria, calcium contents 831ppb, Mg content 12ppb, silicone content 0.96ppm.
embodiment 3
As shown in Figure 1, generated by polyvinyl chloride by calcium carbide peace and quiet thin stillage recycling caustic soda primary brine technique, it comprises the steps:
1) in 20L double-layer glass reaction kettle, add 5L and be taken to generated by polyvinyl chloride by calcium carbide acetylene cleaning workshop section composite 80% and through the peace and quiet waste liquid (in the peace and quiet waste liquid after process, COD is 130mg/L) of Air Exposure, wherein available chlorine content is almost nil; Add 40mL chlorine bleach liquor, wherein available chlorine content is 0.08% after testing, with salt acid for adjusting pH value to 5, and reaction 30min; PH to 12 is regulated again, reaction 60min, filtering-depositing with sodium hydroxide solution; Described hydrochloric acid is selected from the hydrochloric acid of production of caustic soda hydrogen chloride synthesis workshop section, and concentration is 30%; Described sodium hydroxide solution is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section, and mass percent concentration is 32%.
2) get filtrate 500mL and rejoin 20L double-layer glass reaction kettle, mix with 12L primary brine, fully stir, be warming up to 65 DEG C, add 1765g solid sodium chloride, be stirred to sodium-chlor and dissolve completely; Described primary brine is selected from the primary brine of production of caustic soda primary brine workshop section, chloride content 110g/L; Described sodium-chlor is selected from production of caustic soda primary brine workshop section raw material solid sodium-chlor, and sodium chloride content is greater than 94%.
3) add sodium hydroxide solution and regulate pH to 12, add the solution with the preparation of 1.5g ferric chloride (FeCl36H2O), reaction 60min; Detection calcium ion content is 193mg/L, adds 125mL sodium carbonate solution, reaction 60min, and precipitate with triumphant membrane filtration, filtrate being reaches the middle product of primary brine Effluent criteria; Described sodium hydroxide solution is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section, and mass percent concentration is 32%; Described ferric chloride (FeCl36H2O) is selected from the ferric chloride (FeCl36H2O) that production of caustic soda primary brine workshop section uses; Described sodium carbonate solution is selected from the sodium carbonate solution of production of caustic soda primary brine workshop section, content 100g/L; Described triumphant film is selected from the HVM film of production of caustic soda primary brine workshop section.
After measured, reach in the middle product of primary brine Effluent criteria, calcium contents 678ppb, Mg content 5.63ppb, silicone content 0.78ppm.
Claims (10)
1. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide is to the technique of caustic soda primary brine, it is characterized in that, comprises the steps:
1) acetylene gas in peace and quiet waste liquid is removed;
2) adding clorox control available chlorine content is 0.06-0.10%, and adding salt acid for adjusting pH value is 2-5, reaction 10-30min;
3) more than sodium hydroxide adjust ph to 12 is added, reaction 30-60min, filtering-depositing;
4) filtrate mixes with caustic soda primary brine, is warming up to 55-65 DEG C, adds sodium-chlor, controls sodium chloride content and is greater than 300g/L; Wherein, described filtrate and the blending ratio of caustic soda primary brine equal the ratio of peace and quiet waste liquid total Water and primary brine total Water;
5) adding sodium hydroxide control ph is 10-12, adds ferric chloride (FeCl36H2O), and the add-on of ferric chloride (FeCl36H2O) is 0.08-0.12g/L, reaction more than 60min;
6) add sodium carbonate, control sodium carbonate relative to the excessive 0.3-0.8g/L of calcium ion, reaction more than 60min;
7) filter, filtrate being reaches the middle product of primary brine Effluent criteria, and wherein calcium magnesium total content is less than 4 PPm, and silicone content is less than 2.3PPm.
2. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, is characterized in that as claimed in claim 1, and in step 1), described peace and quiet waste liquid is the useless chlorine bleach liquor that generated by polyvinyl chloride by calcium carbide acetylene cleaning workshop section produces.
3. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, is characterized in that as claimed in claim 1, and in step 1), in the peace and quiet waste liquid after removing acetylene gas, COD is 100-150mg/L.
4. as claimed in claim 1 the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide to the technique of caustic soda primary brine, it is characterized in that, step 2) in, described clorox adds with its solution form, and is selected from the chlorine bleach liquor of caustic soda synthesizing section tail chlorine absorption tower generation.
5. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, is characterized in that, step 2 as claimed in claim 1) in, described hydrochloric acid is selected from the hydrochloric acid of production of caustic soda hydrogen chloride synthesis workshop section.
6. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, is characterized in that as claimed in claim 1, step 3) and 5) in, described sodium hydroxide adds with its solution form, and is selected from the sodium hydroxide solution of production of caustic soda finished product workshop section.
7. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, is characterized in that as claimed in claim 1, and in step 4), described primary brine is selected from the primary brine of production of caustic soda primary brine workshop section, chloride content 90-110g/L.
8. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, is characterized in that as claimed in claim 1, and in step 4), described sodium-chlor is selected from production of caustic soda raw material solid sodium-chlor.
9. as claimed in claim 1 the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide to the technique of caustic soda primary brine, it is characterized in that, in step 5), described ferric chloride (FeCl36H2O) adds with its solution form, and is selected from the ferric chloride (FeCl36H2O) of production of caustic soda primary brine workshop section use.
10. the peace and quiet thin stillage recycling of generated by polyvinyl chloride by calcium carbide, to the technique of caustic soda primary brine, is characterized in that as claimed in claim 1, and in step 6), described sodium carbonate adds with its solution form, and is selected from the sodium carbonate solution of production of caustic soda primary brine workshop section.
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