CN102583813B - Recovery method for terephthalic acid in alkali deweighting wastewater as well as production method and application of terephthalic acid metal salt whisker - Google Patents
Recovery method for terephthalic acid in alkali deweighting wastewater as well as production method and application of terephthalic acid metal salt whisker Download PDFInfo
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Abstract
The invention relates to a recovery method for terephthalic acid in alkali deweighting wastewater as well as a production method and application of terephthalic acid metal salt whisker. The recovery method comprises the following steps of: regulating pH value of the wastewater to 10-11, after basic aluminum chloride is added, quickly stirring wastewater at 350-550 r/min for 5-10min, then slowly stirring at 80-120 r/min for 5-10min to obtain wastewater containing floccules, filtering out precipitate from the wastewater containing floccules through waste coal cinder, then adding activated carbon into the wastewater to adsorb for 5-10min, filtering out the activated carbon via one layer of waste coal cinder, stirring wastewater at 80-150 r/min for 5-10min, simultaneously adding dilute sulphuric acid or hydrochloric acid into the wastewater, when the pH value of the wastewater is lowered to 3-4, and ageing for 1-5h in an ageing pool to obtain crude terephthalic acid of which the purity is 95%. The whisker-shaped terephthalic acid metal salt, which is obtained by taking terephthalic acid recovered from the alkali deweighting wastewater as a raw material, can serve as an active filler of rubber to enhance rubber product performance.
Description
Technical field
The present invention relates to production method and the application of recovery method and terephthaldehyde's acid metal salt whisker of terephthalic acid in alkali decrement waste water
Background technology
Whisker refers to a kind of fiber that grows into high purity monocrystalline form under the manual control condition, therefore has excellent mechanical property.Due to its courtyard structural arrangement high-sequential, structural integrity is difficult to hold the defect that lives forever in macrocrystal,, so physical strength is approximately equal to the theoretical strength of valence link power between atom, is very excellent advanced composite material strengthening and toughening material.
Along with the fast development of China's polyester chemical fibre industry, the alkali Decrement Technique has been widely used in the production of the products such as Silk, Super-fine Synthetic Leather, and that the alkali decrement waste water that produces has therefrom become is harmful, one of unmanageable trade effluent.Alkali decrement waste water contains a large amount of terephthalic acids (approximately 60%), fiber degradation by product and caustic soda, general pH＞13, and CODcr is at 2000～80000mg/L, and not biodegradable solvability COD is at 600～1000mg/L.The characteristics of this type of waste water are: basicity is large, pollutant load is high, biodegradability is poor, belong to high concentration hard-degraded organic waste water, it is almost impossible only depending on biological process to deal with problem, and the COD that reduces waste water by materialization can bring a large amount of body refuses, to environment, causes secondary pollution.Therefore, explore practical, economic alkali decrement waste water treatment process extremely urgent.
Method commonly used is first alkali decrement waste water to be carried out pre-treatment at present, reclaims terephthalic acid and carries out biochemical treatment afterwards again.Although it is a lot of to reclaim the method for terephthalic acid, several major parts are based on direct acid-precipitation method, though this method has certain utility value, but the terephthalic acid that reclaims is impure more, content is generally in 75% left and right, and purity is lower, directly causes its Application Areas and range limited.Therefore, but the technique of a kind of not only economical and practical but also efficient recovery terephthalic acid need to be provided, the requirement that waste water resource is recycled could be met.The technique of research terephthaldehyde acid recovery purifying has had much at present:
Publication number is method and the device that the Chinese invention patent application of CN1680262 discloses a kind of integrated basic decrement waste water reclamation terephthalic acid, what this invention was mainly adopted is that alkali decrement waste water and sulfuric acid add from tank body top entrance respectively simultaneously continuously, the pH value that controller generates mixture solution at first is 4-7, again appropriate sulfuric acid is supplemented and adds from the tank body middle part, make pH value of solution to 2-3, then mixture solution is put into whizzer and separated from tank is low, make crude terephthalic acid.
Publication number is the method for purification that the Chinese invention patent of CN1680261 discloses a kind of crude terephthalic acid, the method is to adopt the device of CN1680262, the crude terephthalic acid that obtains is further dried the ball milling screening, then under 60 ℃～100 ℃, be dipped in water, stir clarification, thereafter low suspension liquid carries out centrifugation, the terephthalic acid of centrifuge dehydration is dried under 80 ℃～105 ℃, can make the higher terephthalic acid finished product of purity, can be used as the raw material of synthetic terylene chips.
Publication number is the treatment process that the Chinese invention patent of CN101244857A discloses a kind of alkali decrement waste water, the method be with alkali decrement waste water the pH value be adjusted to 6.5～7, carry out acid out and obtain containing the solution of terephthalic acid, the gained terephthalic acid is carried out esterification under methyl alcohol exists, obtain the thick product of dimethyl terephthalate (DMT).
But these patents reclaim the terephthalic acid that obtains substantially all is used for raw material or production dimethyl terephthalate (DMT) as synthetic terylene chips, and the not high reason of product purity that obtains due to recovery, causes these techniques not obtain industrial applications.
Technology contents
The technical problem to be solved in the present invention is that the terephthalic acid purity of existing alkali decrement process for waste water processing extraction is low, and Application Areas is restricted.
One object of the present invention is to obtain to make terephthalic acid can become the method for good renewable resource, the method reclaims terephthalic acid from alkali decrement waste water, make the CODcr value of waste water descend more than 75%, and the crude terephthalic acid purity 95% that obtains.
Another object of the present invention is to obtain a kind of production method of terephthaldehyde's acid metal salt, the method can prepare terephthaldehyde's acid metal salt of crystal whisker-shaped take the terephthalic acid that reclaims in alkali decrement waste water as raw material, can be used as the active filler of rubber, the reinforcing rubber articles performance.
First part of the present invention content, provide a kind for the treatment of process of alkali decrement waste water, comprises the steps:
the pH value to 10 of adjusting waste water～11, add the aluminium chlorohydroxide that accounts for wastewater quality 5%～20%, rear waste water first passes through 350-550 rev/min, the rapid stirring of 5-10min, by 80-120 rev/min, the low rate mixing of 5-10min, obtain containing the waste water of throw out through waste coal slag filtering precipitate, afterwards again toward the gac that adds 10%～30% in waste water, after absorption 5～10min, filter out gac through one deck waste coal slag blanket again, with 80 rev/mins～150 rev/mins, 5-10min stirs waste water, simultaneously add dilute sulphuric acid or hydrochloric acid in waste water, treat that waste water ph is down to 3～4, at ageing pond ageing 1～5h, the purity 95% of the crude terephthalic acid that obtains.
The second part of the present invention, provide a kind of production method of terephthaldehyde's acid metal salt whisker, comprises the steps:
Add caustic soda soln again to dissolve resulting crude terephthalic acid, regulate the pH value 6～8, add polyol-based non-ionic surfactant, stirring and evenly mixing, then add soluble calcium salt (as CaCl
2Deng), stirring, ageing 1～5h, can obtain terephthaldehyde's acid metal salt whisker.
The crude terephthalic acid of producing terephthaldehyde's acid metal salt whisker is the terephthalic acid that reclaims in alkali decrement waste water.
Technique effect of the present invention is to efficiently solve that alkali decrement waste water is difficult to carry out a biological disposal upon and the printing and dyeing comprehensive wastewater that causes due to the reason of alkali decrement waste water changes unpredictably, processes the difficult problem that parameter strengthens, " secondary pollution " effect that a large amount of body refuses that solved again simultaneously materialization processing alkali decrement waste water and produced produce environment, can only landfill or the body refuse of burning turn waste into wealth, become industrial reusable raw material, create certain economic benefit.On the one hand the AT raw material of recovery is utilized again, can reduce on the other hand the processing load of residue waste water, solve the high problem of processing costs, environmental benefit and economic benefit are taken into account, and improve simultaneously processing efficiency, environmental contamination reduction.The present invention has prepared a kind of whisker of terephthaldehyde's acid metal salt on the other hand, and this whisker improves a lot to its mechanical property after adding the rubber plastic material.
Description of drawings
The SEM figure of Fig. 1 embodiment 1
The XRD figure of Fig. 2 embodiment 1
The SEM figure of Fig. 3 embodiment 5
The SEM figure of Fig. 4 embodiment 6
Specific embodiment and accompanying drawing
Embodiment 1: the pH value to 11 of regulating waste water, add 20% aluminium chlorohydroxide, rear waste water is first through 500 rev/mins, the rapid stirring of 6min, by 100 rev/mins, the low rate mixing of 6min, obtain containing the waste water of throw out through waste coal slag filtering precipitate, afterwards again toward the gac that adds 30% in waste water, after absorption 10min, filter out gac through one deck waste coal slag blanket again, stir waste water with 150 rev/mins, 6min, add dilute sulphuric acid simultaneously in waste water, treat that waste water ph is down to 3, at ageing pond ageing 5h, the crude terephthalic acid that obtains.After testing, wherein the purity of terephthalic acid reaches 95%.
The crude terephthalic acid that embodiment 1 is obtained adds caustic soda soln again to dissolve, and regulates the pH value 8, adds the polyoxyethylene glycol nonionogenic tenside, stirring and evenly mixing, then add soluble metallic salt CaCl
2, stirring, ageing 5h, can obtain the terephthalic acid calcium pyroborate.Can find out from Fig. 1 and 2, terephthaldehyde's acid metal salt that the inventive method prepares is the whisker of fibrous texture.
Embodiment 2: the pH value to 10 of regulating waste water, add 5% aluminium chlorohydroxide, rear waste water is first through 350 rev/mins, the rapid stirring of 10min, by 120 rev/mins, the low rate mixing of 5min, obtain containing the waste water of throw out through waste coal slag filtering precipitate, afterwards again toward the gac that adds 10% in waste water, after absorption 5, filter out gac through one deck waste coal slag blanket again, stir waste water with 80 rev/mins, 10min, add hydrochloric acid simultaneously in waste water, treat that waste water ph is down to 3, in ageing pond ageing 1, the purity 95% of the crude terephthalic acid that obtains.
Add caustic soda soln again to dissolve resulting crude terephthalic acid, regulate the pH value 6, add Determination of Polyoxyethylene Non-ionic Surfactants, stirring and evenly mixing, then add soluble metallic salt MgCl
2, to stir, ageing 1, can obtain terephthalic acid magnesium whisker.
Embodiment 3: the pH value to 10 of regulating waste water, add 13% aluminium chlorohydroxide, rear waste water is first through 550 rev/mins, the rapid stirring of 5min, by 80 rev/mins, the low rate mixing of 10min, obtain containing the waste water of throw out through waste coal slag filtering precipitate, afterwards again toward the gac that adds 20% in waste water, after absorption 8min, filter out gac through one deck waste coal slag blanket again, stir waste water with 130 rev/mins, 5min, add hydrochloric acid simultaneously in waste water, treat that waste water ph is down to 3, at ageing pond ageing 3h, the purity 95% of the crude terephthalic acid that obtains.
Add caustic soda soln again to dissolve resulting crude terephthalic acid, regulate the pH value 7, add polyoxyethylene-type or polyol-based non-ionic surfactant, stirring and evenly mixing, then add soluble metallic salt ZnCl
2, stirring, ageing 3h, can obtain terephthalic acid zinc whisker.
Embodiment 4: the pH value to 11 of regulating waste water, add 20% aluminium chlorohydroxide, rear waste water is first through 300 rev/mins, the stirring of 6min, and the waste water that obtains containing throw out is through waste coal slag filtering precipitate, afterwards again toward the gac that adds 30% in waste water, after absorption 10min, filtering out gac through one deck waste coal slag blanket again, with 150 rev/mins, 6min, stir waste water, is the dilute sulphuric acid of 10ppm toward adding concentration in waste water simultaneously, treat that waste water ph is down to 3, obtain crude terephthalic acid.After testing, wherein the purity of terephthalic acid reaches 80%.
Embodiment 5: the crude terephthalic acid that embodiment 1 is obtained adds soluble metallic salt CaCl after dissolving with caustic soda
2, the sedimentation and filtration oven dry that obtains.Fig. 3 shows that the terephthaldehyde's acid metal salt that adopts this technique to prepare is very common crystalline particulate, but not whisker.
Embodiment 6: add caustic soda soln again to dissolve the resulting crude terephthalic acid of embodiment 1, regulate the pH value 7, add the non-ion fluorin carbon surface active agent, stirring and evenly mixing, then add soluble metallic salt ZnCl
2, stirring, ageing 3h, obtain terephthalic acid calcium.Fig. 4 shows that the terephthaldehyde's acid metal salt that adopts this technique to prepare is very common crystalline particulate, but not whisker.
Embodiment 7: with the crystal whisker materials of embodiment 1-3 gained (experiment 1-3), traditional packing material CaCO
3(experiment 4), embodiment 5 gained terephthalic acid calcium (experiment 5) and high density polyethylene blend, mass ratio is 30%:70%, makes plastic tab, carries out correlation detection.The national standard of each measured performance parameter method institute foundation is specific as follows: tensile strength is pressed GB/T 1701-2001 and is measured, elongation at break is pressed GB/T 1701-2001 and is measured, color and luster, peculiar smell, differently smell, foreign matter adopts appearance method, aging velocity of variation press GB/T 16585-1996 mensuration.Detect data such as following table 1:
Table 1
Measure the CODcr value of initial waste water and the waste water after embodiment 1 (No. 1 waste water), embodiment 4 (No. 2 waste water) are processed, adopt quick potassium dichromate oxidation one ferrous sulfate titration measuring:
| Initial waste water | No. 1 waste water | No. 2 waste water | |
| The CODcr value | 1015mg/L | 235mg/L | 250mg/L |
| The CODcr clearance | - | 76.8％ | 75.3％ |
Take above-mentioned foundation desirable embodiment of the present invention as enlightenment, by above-mentioned description, the relevant staff can in the scope that does not depart from this invention technological thought, carry out various change and modification fully.The technical scope of this invention is not limited to the content on specification sheets, must determine its technical scope according to the claim scope.
Claims (1)
1. method of producing terephthaldehyde's acid metal salt whisker, it is characterized in that: described method is for adding crude terephthalic acid caustic soda soln to dissolve, regulate the pH value 6～8, add the polyoxyethylene glycol nonionogenic tenside, stirring and evenly mixing, then add soluble calcium salt, stir, ageing 1～5h, can obtain terephthaldehyde's acid metal salt whisker
wherein, crude terephthalic acid is that the processing by alkali decrement waste water gets, concrete treatment process is, the pH value to 10 of adjusting alkali decrement waste water～11, add the aluminium chlorohydroxide that accounts for wastewater quality 5%～20%, rear waste water first passes through 350-550 rev/min, the rapid stirring of 5-10min, by 80-120 rev/min, the low rate mixing of 5-10min, obtain containing the waste water of throw out through waste coal slag filtering precipitate, afterwards again toward the gac that adds 10%～30% in waste water, after absorption 5～10min, filter out gac through one deck waste coal slag blanket again, with 80 rev/mins～150 rev/mins, 5-10min stirs waste water, simultaneously add dilute sulphuric acid or hydrochloric acid in waste water, treat that waste water ph is down to 3～4, at ageing pond ageing 1～5h, the purity of the crude terephthalic acid that obtains reaches 95%.
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| CN106977063A (en) * | 2017-06-01 | 2017-07-25 | 常州市五洲环保科技有限公司 | Alkali decrement waste water deep treatment method |
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| JPS6143140A (en) * | 1984-08-07 | 1986-03-01 | Johoku Kagaku Kogyo Kk | Method of recovering high-purity terepthalic acid from terephthalic acid-containing waste liquir |
| KR920000416B1 (en) * | 1989-10-13 | 1992-01-13 | 재단법인 한국화학연구소 | Process for preparing for high quality terephthalic acid |
| CN1686871A (en) * | 2005-04-23 | 2005-10-26 | 陈一鸣 | Method for preparing antiager from wastewater of alkali weight reduction |
| CN101148298A (en) * | 2007-09-11 | 2008-03-26 | 浙江大学 | Integration treatment recovery method for alkali decrement waste water by film method |
| CN201424412Y (en) * | 2009-06-18 | 2010-03-17 | 江苏尚宝罗泵业有限公司 | Alkali-reduction wastewater processing system |
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