CN106977063A - Alkali decrement waste water deep treatment method - Google Patents
Alkali decrement waste water deep treatment method Download PDFInfo
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- CN106977063A CN106977063A CN201710405304.XA CN201710405304A CN106977063A CN 106977063 A CN106977063 A CN 106977063A CN 201710405304 A CN201710405304 A CN 201710405304A CN 106977063 A CN106977063 A CN 106977063A
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- waste water
- clear liquid
- alkali decrement
- rotating speed
- decrement waste
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
- C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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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
- C02F3/00—Biological treatment of water, waste water, or sewage
Abstract
The invention discloses a kind of alkali decrement waste water deep treatment method, comprise the following steps：（1）The pH value of waste water is adjusted to 10~11, aluminium chloride is added, 3 10min is stirred under 400 800rpm rotating speed, then 10 20min are mixed slowly under 100 300rpm rotating speed, suspension is through cinder filtration, and filtrate passes through active carbon filter again, obtains clear liquid；（2）Clear liquid is reacted with soluble metal salt saturated solution in ultrasound-enhanced tubular reactor, discharging is through separation of solid and liquid, it can be used after filter cake drying as the functional aid of rubber-plastics material, go out filter liquor and enter biochemical treatment system, further handle rear discharge up to standard or reuse.The present invention can make the CODcr value reduced rates of alkali decrement waste water more than 82%, biodegradability raising；Meanwhile, thinner, the metal purity salt evenly that crystallization is separated out reaches more than 99.5%, has more excellent feature in rubber-plastics material.
Description
Technical field
The present invention relates to a kind of alkali decrement process for waste water processing, and in particular to one kind utilizes ultrasound-enhanced crystallization reaction depth
Remove Coal Gas Washing Cycling Water organic matter, improve the deep treatment method of water outlet biodegradability.
Background technology
With developing rapidly for China's polyester chemical fibre industry, Alkali reduction technology has been widely used in Silk, ultra-fine conjunction
In the production of the products such as finished leather.Polyester fiber（PET）Under low temperature, without obvious chemical action in dilute NaOH solution, and highly concentrated
Spend under NaOH solution and higher temperature, PET and NaOH plays hydrolysis generation para-phthalic sodium (TA-Na) and ethylene glycol
(EG) the weightless decrements of PET, are made, hydrolysis decrement is general 3.5%~30%, that is, the PET for having 3.5%~30% is present in buck
In.From the PET that stripping is dissolved on dacron enters water, the overwhelming majority exists with TA-Na and EG states of matter, on a small quantity with difference
The oligomer of the degree of polymerization is present.It is general per 30 ~ 50 tons of myriametre woven dacron decrement discharge waste water, CODcr at concentrations up to tens thousand of mg/L,
Although the water only accounts for a few percent of dyeing and finishing composite waste to more than ten percent, mono- pollutant of the TA-Na discharged is just
The 40%~78% of total CODcr is accounted for, oneself turns into the difficult point and emphasis of current textile printing and dyeing industry environment protection treating to this effluent part, because
This, alkali decrement waste water remerges processing after should individually pre-processing.The conventional way of PET industry is first pre- to waste water progress acid out
Processing, removes TA-Na, then carries out biochemical treatment, i.e., using the biochemical combined treatment process of materialization one.
It is an effective method that acid-precipitation method, which removes TA-Na in alkali decrement waste water, but is also primarily present both sides problem：
（1）The waste water COD clearance of acid out processing is limited, and the load of subsequent biochemical processing is still larger；（2）The solid waste TA that acid out is reclaimed is pure
The poor, particle of degree is tiny, dehydration property is poor, no reuse value, burns or landfill disposal also easily causes secondary pollution.
Publication No. CN105731699 patent of invention discloses terephthaldehyde in a kind of resource reutilization alkali decrement waste water
The method of acid.The metal salt of terephthalic acid purity reclaimed using this method is high, available in the modification of product of rubber and plastic；Extraction pair
Waste water post processing load reduction after phthalic acid metal salt, the problem of solving processing cost and high cost of investment, Environmental Effect
Benefit and economic benefit are taken into account.This method can make the CODcr values of alkali decrement waste water decline more than 75%.
Publication No. CN1935703 patent of invention discloses one kind and reclaims terephthalic acid (TPA) from colored alkali decrement waste water
Technique, the dense dilute two strands of waste water dual treatments produced to caustic reduction processing are first decolourized using decolorising agent, then pass through acid
Analysis method is combined with embrane method, and terephthalic acid (TPA) is reclaimed from alkali decrement waste water, is made the CODcr values of waste water and is reduced by 50% ~ 70%, is easy to
Follow-up biochemistry, materializing strategy.
Publication No. CN103755555 patent of invention discloses the smart terephthaldehyde of one kind alkali decrement waste water residue production
The device of acid, by reclaiming residue from alkali decrement waste water, while alkali decrement waste water residue is changed into p-phthalic acid's production
Product so that the CODcr values clearance of alkali decrement waste water is up to 75% or so.
The CODcr of alkali decrement waste water after being handled using above method has different degrees of reduction.If alkali can be improved
The handling process of decrement waste water, makes CODcr decreasing value higher, it will the load that further reduction waste water subsequent biochemical is handled.
The content of the invention
The invention provides a kind of deep treatment method of alkali decrement waste water so that water outlet CODcr values reduced rate 82% with
Upper, biodegradability is improved.Meanwhile, thinner, the terephthalic acid (TPA) calcium evenly that crystallization is separated out（TA-Ca）Or terephthalic acid (TPA) zinc
（TA-Zn）, purity reaches more than 99.5%, with more excellent feature in rubber-plastics material.
To achieve these goals, the present invention is achieved through the following technical solutions：A kind of alkali decrement waste water of the present invention
Deep treatment method, comprises the following steps：
Step one：The pH value of waste water is adjusted to 10~11, aluminium chloride is added, 3- is stirred under 400-800rpm rotating speed
10min, then 10-20min is mixed slowly under 100-300rpm rotating speed, suspension is through cinder filtration, and filtrate is again by activity
Carbon filter, obtains clear liquid.
Step 2：Clear liquid is reacted with soluble metal salt saturated solution in ultrasound-enhanced tubular reactor, discharging
Through separation of solid and liquid, it can be used after filter cake drying as the functional aid of rubber-plastics material, go out filter liquor and enter biochemical treatment system,
Further handle rear discharge up to standard or reuse.
Further, the mol ratio of TA-Na and soluble metallic salt is preferably 1 in clear liquid:1~1:1.1.
Described soluble metallic salt is calcium, the ease of solubility salt of zinc.
The application frequency of the ultrasonic wave is 55 ~ 75KHz, and power is 400 ~ 600W.
The present invention carries out advanced treating by simple, easy method to alkali decrement waste water, compared with prior art, has
Following advantage：
（1）In the presence of ultrasound-enhanced, the reaction between TA-Na and soluble metallic salt can be reduced so that the TA-Na energy in water
TA-Ca or TA-Zn is more fully converted into, water outlet CODcr reduced rate reaches more than 82%
（2）In ultrasound-enhanced tubular reactor, the TA-Ca or TA-Zn that crystallization is obtained during flow forward constantly
Dissolving, recrystallization, further increase TA-Na conversion ratio, while obtained TA-Ca or TA-Zn granularities are more carefully, evenly,
Purity can reach more than 99.5%.
Brief description of the drawings
Fig. 1 is TA-Ca prepared by embodiment 1 particle size distribution figure.
Fig. 2 is TA-Zn prepared by embodiment 2 particle size distribution figure.
Fig. 3 is TA-Ca prepared by embodiment 4 particle size distribution figure.
Fig. 4 is TA-Zn prepared by embodiment 5 particle size distribution figure.
Embodiment
The present invention is further illustrated by the following examples.It should be understood that these embodiments are the explainations of the present invention
And citing, the scope of the present invention is not limited in any form.
Embodiment 1
Step one：The pH value of waste water is adjusted to 10, aluminium chloride is added, 10min is stirred under 400 rpm rotating speed, then
20min is mixed slowly under 100 rpm rotating speed, suspension is through cinder filtration, and filtrate passes through active carbon filter again, obtain clear
Liquid.
Step 2：Clear liquid is reacted with calcium chloride saturated solution in ultrasound-enhanced tubular reactor, is discharged through solid-liquid
Separation, can use as the functional aid of rubber-plastics material after filter cake drying, go out filter liquor and enter biochemical treatment system, further
Discharge or reuse after processing is up to standard.
The mol ratio of TA-Na and calcium chloride is 1 in the clear liquid:1.
The application frequency of the ultrasonic wave is 55KHz, and power is 400W.
CODcr detections are carried out to the filter liquor that goes out of step 2,1 is the results are shown in Table；Calcium content point is carried out to prepared TA-Ca
Analysis, the results are shown in Table 2；TA-Ca particle size distribution figure is shown in Fig. 1.
Embodiment 2
The difference of embodiment 2 and embodiment 1 is：
In step one, the pH value of waste water is adjusted to 11, aluminium chloride is added, 3min is stirred under 800rpm rotating speed, then
10min is mixed slowly under 300rpm rotating speed.
In step 2, clear liquid is reacted with zinc chloride saturated solution in ultrasound-enhanced tubular reactor.
The mol ratio of TA-Na and zinc chloride is 1 in the clear liquid:1.1.
The application frequency of the ultrasonic wave is 75KHz, and power is 600W.
CODcr detections are carried out to the filter liquor that goes out of step 2,1 is the results are shown in Table；Zn content point is carried out to prepared TA-Zn
Analysis, the results are shown in Table 2；TA-Zn particle size distribution figure is shown in Fig. 2.
Embodiment 3
The difference of embodiment 3 and embodiment 1 is：
In step one, the pH value of waste water is adjusted to 10.5, aluminium chloride is added, 7min is stirred under 600rpm rotating speed,
Again 15min is mixed slowly under 200rpm rotating speed.
In step 2, clear liquid is reacted with calcium nitrate saturated solution in ultrasound-enhanced tubular reactor.
The mol ratio of TA-Na and calcium nitrate is 1 in the clear liquid:1.05.
The application frequency of the ultrasonic wave is 65KHz, and power is 500W.
CODcr detections are carried out to the filter liquor that goes out of step 2,1 is the results are shown in Table.
Comparative example 1
The difference of comparative example 1 and embodiment 1 is：
In step 2, added into clear liquid and account for the soluble calcium chloride saturated solution of wastewater quality 0.05%, with 1000 turns/min
Speed quickly stir after 2min, add great amount of soluble calcium chloride saturated solution, vibrated using low frequency ultrasound, to clear liquid pH
Value is down to after 8, separation of solid and liquid, can be used after filter cake drying as the functional aid of rubber-plastics material, is gone out filter liquor and is entered biochemical
Processing system, further handles rear discharge up to standard or reuse.
CODcr detections are carried out to going out filter liquor, 1 is the results are shown in Table；Calcium content analysis is carried out to prepared TA-Ca, as a result
It is shown in Table 2；TA-Ca particle size distribution figure is shown in Fig. 3.
Comparative example 2
The difference of comparative example 2 and embodiment 2 is：
In step 2, added into clear liquid and account for the soluble chlorination zincification solution of wastewater quality 0.05%, with 1000 turns/min
Speed quickly stir after 2min, add great amount of soluble zinc chloride saturated solution, vibrated using low frequency ultrasound, to clear liquid pH
Value is down to after 8, separation of solid and liquid, can be used after filter cake drying as the functional aid of rubber-plastics material, is gone out filter liquor and is entered biochemical
Processing system, further handles rear discharge up to standard or reuse.
CODcr detections are carried out to going out filter liquor, 1 is the results are shown in Table；Zn content analysis is carried out to prepared TA-Zn, as a result
It is shown in Table 2；TA-Zn particle size distribution figure is shown in Fig. 4.
Comparative example 3
Acid out processing is carried out to alkali decrement waste water with sulfuric acid, when pH is down to 2.5-3.5, separation of solid and liquid is carried out, goes out filter liquor and enter
Enter biochemical treatment system, further handle rear discharge up to standard or reuse.
CODcr detections are carried out to going out filter liquor, 1 is the results are shown in Table.
Experiment 1
The CODcr of water sample is detected according to standard HJ 828-2017 method, and calculates corresponding CODcr reduced rates, testing result
It is shown in Table 1.
Experiment 2
（1）The method of testing of ash content
Content of ashes is tested according to the detection method of ash content in standard 11409-2008, testing result is shown in Table 2.
（2）The method of testing of Zn content
Weigh certain amount above-mentioned（1）Obtained ash content, after dissolving with hydrochloric acid, adjusts the pH of solution, using xylenol orange as instruction
Agent, with EDTA solution titrimetry Zn contents, testing result is shown in Table 2.
（3）The method of testing of calcium content
Weigh certain amount above-mentioned（1）Obtained ash content, after dissolving with hydrochloric acid, adjusts the pH of solution, using calcium carboxylate as indicator,
With EDTA solution titrimetry calcium contents, testing result is shown in Table 2.
Experiment 3
TA-Ca or TA-Zn made from embodiment and comparative example are applied in tire tread formula, formula used is：NR 100、
Stearic acid 2, zinc oxide 4, N220 35, white carbon 8, Si69 0.8, aromatic naphtha 5, protection wax 2,4010NA 1.5, sulphur
Sulphur 1.2, NOBS 1.6, functional form auxiliary agent（Become kind, TA-Ca made from embodiment 1, TA-Zn, contrast made from embodiment 1
TA-Ca made from example 1, TA-Zn made from comparative example 2,） 10.
In two-roll mill, first natural rubber is plasticated, various auxiliary agents are then added, elastomeric compound is obtained, then
Vulcanized at 151 DEG C by sulfurizing time, obtain vulcanizing rubber.Tested by national standard, gained performance is shown in Table 3.
The CODcr testing results of table 1
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Influent COD cr, mg/L | 20540 | 20540 | 20540 | 20540 | 20540 | 20540 |
| Water outlet CODcr, mg/L | 3472 | 3390 | 3286 | 4457 | 4519 | 6175 |
| CODcr reduced rates, % | 83.1 | 83.5 | 84.0 | 78.3 | 78.0 | 70.0 |
Find out from the data comparison of table 1：The CODcr reduced rates of alkali decrement waste water after being handled using the method for present specification are more
It is high.
The terephthalate purity analysis result of table 2
| Index | Embodiment 1 | Embodiment 2 | Comparative example 1 | Comparative example 2 |
| Ash content, % | 27.37 | 35.24 | 26.73 | 34.66 |
| Calcium content, % | 19.55 | — | 19.12 | — |
| Zn content, % | — | 28.27 | — | 27.87 |
| TA-Ca ideal calciums, % | 19.61 | — | 19.61 | — |
| TA-Zn theory Zn contents, % | — | 28.38 | — | 28.38 |
| Purity, % | 99.7 | 99.6 | 97.5 | 98.2 |
It is compared with the calcium or Zn content that detect with theoretical value, gap is smaller, illustrates the TA-Ca and TA-Zn of preparation
Purity is higher.Find out from the data comparison of table 2：The TA-Ca and TA-Zn purity prepared using the method for present specification is higher.
The performance data of table 3
Find out from the correction data of table 3：The TA-Ca and TA-Zn prepared using the method for present specification is applied in rubber compounding
In, make vulcanizate that there is more excellent mechanical performance and ageing properties.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, the present invention
Claimed scope is by appended claims, specification and its equivalent thereof.
Claims (4)
1. a kind of alkali decrement waste water deep treatment method, it is characterised in that comprise the following steps：
Step one：The pH value of waste water is adjusted to 10~11, aluminium chloride is added, 3- is stirred under 400-800rpm rotating speed
10min, then 10-20min is mixed slowly under 100-300rpm rotating speed, suspension is through cinder filtration, and filtrate is again by activity
Carbon filter, obtains clear liquid；
Step 2：Clear liquid is reacted with soluble metal salt saturated solution in ultrasound-enhanced tubular reactor, and discharging is through solid
Liquid is separated, and can be used after filter cake drying as the functional aid of rubber-plastics material, be gone out filter liquor and enter biochemical treatment system, enter one
Discharge or reuse after step processing is up to standard.
2. processing method as claimed in claim 1, it is characterised in that the mol ratio of TA-Na and soluble metallic salt is preferred in clear liquid
For 1:1~1:1.1.
3. processing method as claimed in claim 1, it is characterised in that described soluble metallic salt is calcium, the ease of solubility salt of zinc.
4. processing method as claimed in claim 1, it is characterised in that the application frequency of the ultrasonic wave is 55 ~ 75KHz, power is
400~600W。
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503353A (en) * | 2009-03-05 | 2009-08-12 | 浙江大学 | Technique for purifying crude terephthalic acid from alkali deweighting wastewater |
| CN102583813A (en) * | 2012-01-12 | 2012-07-18 | 江苏爱特恩高分子材料有限公司 | Recovery method for terephthalic acid in alkali deweighting wastewater as well as production method and application of terephthalic acid metal salt whisker |
| CN104671506A (en) * | 2015-03-03 | 2015-06-03 | 常州市博洋新材料科技有限公司 | Method for extracting terephthalic acid from alkali-decrement wastewater |
| CN105731699A (en) * | 2016-02-15 | 2016-07-06 | 常州市五洲化工有限公司 | Method for recycling terephthalic acid in alkali-minimization wastewater in resource mode |
| CN105753687A (en) * | 2016-02-15 | 2016-07-13 | 常州市五洲化工有限公司 | Method for acquiring large-particle terephthalic acid crystals from alkali peeling wastewater |
-
2017
- 2017-06-01 CN CN201710405304.XA patent/CN106977063A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503353A (en) * | 2009-03-05 | 2009-08-12 | 浙江大学 | Technique for purifying crude terephthalic acid from alkali deweighting wastewater |
| CN101503353B (en) * | 2009-03-05 | 2012-05-09 | 浙江大学 | Technique for purifying crude terephthalic acid from alkali deweighting wastewater |
| CN102583813A (en) * | 2012-01-12 | 2012-07-18 | 江苏爱特恩高分子材料有限公司 | Recovery method for terephthalic acid in alkali deweighting wastewater as well as production method and application of terephthalic acid metal salt whisker |
| CN102583813B (en) * | 2012-01-12 | 2013-11-13 | 江苏爱特恩高分子材料有限公司 | Recovery method for terephthalic acid in alkali deweighting wastewater as well as production method and application of terephthalic acid metal salt whisker |
| CN104671506A (en) * | 2015-03-03 | 2015-06-03 | 常州市博洋新材料科技有限公司 | Method for extracting terephthalic acid from alkali-decrement wastewater |
| CN105731699A (en) * | 2016-02-15 | 2016-07-06 | 常州市五洲化工有限公司 | Method for recycling terephthalic acid in alkali-minimization wastewater in resource mode |
| CN105753687A (en) * | 2016-02-15 | 2016-07-13 | 常州市五洲化工有限公司 | Method for acquiring large-particle terephthalic acid crystals from alkali peeling wastewater |
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| 沈玉龙等: "《绿色化学（第三版）》", 31 July 2016, 中国环境出版社.北京 * |
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