CN105753687B - A method of obtaining bulky grain terephthalic acid crystals from alkali decrement waste water - Google Patents
A method of obtaining bulky grain terephthalic acid crystals from alkali decrement waste water Download PDFInfo
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- CN105753687B CN105753687B CN201610086445.5A CN201610086445A CN105753687B CN 105753687 B CN105753687 B CN 105753687B CN 201610086445 A CN201610086445 A CN 201610086445A CN 105753687 B CN105753687 B CN 105753687B
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- 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
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
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- C07B2200/13—Crystalline forms, e.g. polymorphs
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Abstract
The method that the present invention relates to a kind of to obtain bulky grain terephthalic acid crystals from alkali decrement waste water.Aluminium chloride is added in waste water, quickly stirs, adjusts the pH value of waste water to 10~11, mix slowly, then through waste coal slag filtering precipitate, adsorbed through active carbon layer, then is filtered through one layer of waste coal slag blanket.The terephthalic acid (TPA) of a small amount of certain mesh number is added into clear liquid, after be slowly added to diluted acid, after clear liquid pH value is down to 2~3, stand 15min, for gained solid-liquid mixture by filter press press filtration, filter residue is washed, drying.Gained terephthalic acid particles are big, and convenient for filtering, purity up to 99% or more, create economic benefit, and reduce environmental pollution by recyclable recycling.
Description
Technical field
The method that the present invention relates to a kind of to obtain bulky grain terephthalic acid crystals from alkali decrement waste water.
Background technology
With the fast development of China's polyester chemical fibre industry, Alkali reduction technology has been widely used for Silk, ultra-fine synthesis
In the productions of products such as leather, the alkali decrement waste water generated therefrom has become one of harmful, intractable industrial wastewater.Alkali reduction
The waste water COD cr values for processing generation are usually tens of thousands of, and the waste water COD cr generated accounts for 50% or more of dyeing waste water CODcr total amounts,
Per myriametre terylene after alkali deweighting process, 30~50 tons of alkali decrement waste waters are discharged, CODcr is up to 20000mg/
L or more need to take 1~2 week or even longer time using biochemical treatment organic matter therein, therefore using at biochemical process
Reason, construction investment is big, and operating cost is high, and water outlet is extremely difficult to discharge standard.Therefore, explore practical, economic alkali decrement waste water
Treatment process is extremely urgent.
Currently used method is first to pre-process alkali decrement waste water, and biochemistry is carried out again after recycling terephthalic acid (TPA)
Processing.Although recycling terephthalic acid (TPA) method it is very much, several major be based on direct acid-precipitation method, though the method has certain profit
With value, but the terephthalic acid (TPA) grain size recycled is small, hardly possible separation, and impure more, and purity is relatively low, cause its application field and
Range is limited.Accordingly, it is desirable to provide technique that is a kind of not only economical and practical but also can effectively recycling terephthalic acid (TPA), could meet waste water
The requirement of resource recycling.
Technology contents
The technical problem to be solved by the present invention is to the terephthalic acid crystals of existing alkali decrement process for waste water processing extraction
Grain is small, and purity is low, and application field is restricted.
It is an object of the present invention to obtain enable terephthalic acid (TPA) become good regenerated resources method, this method from
Terephthalic acid (TPA) is recycled in alkali decrement waste water so that the CODcr values of waste water decline 75% or more, and the crude terephthalic acid obtained
Purity is up to 99% or more, and grain size is in 50um or more, convenient subsequently separation of solid and liquid and the recycling of product.
The present invention provides a kind of processing methods of alkali decrement waste water, include the following steps：
Step 1: the aluminium chloride for accounting for wastewater quality 5%~20% is added in waste water, quickly stirs, adjust waste water
PH value is mixed slowly to 10~11, then through waste coal slag filtering precipitate, and clear liquid is adsorbed through active carbon layer, then through one layer of waste coal slag
Layer filtering.
Step 2: the terephthalic acid (TPA) powder for 500 mesh of the mistake sieve for accounting for wastewater quality 0.05%~1% is added into clear liquid
End, after be slowly added to diluted acid, after clear liquid pH value is down to 2~3, stand 15min, gained solid-liquid mixture passes through filter press pressure
Filter, filter residue is washed, drying.Gained terephthalic acid particles are big, and convenient for filtering, purity is up to 99% or more, recyclable recycling.
The terephthalic acid powder was preferably the powder of 800 mesh sieve.
The solution have the advantages that efficiently solving alkali decrement waste water is difficult to biological treatment and due to alkali decrement waste water
Dyeing synthetic wastewater caused by reason changes unpredictably, handles the problem of parameter increasing, while solving materializing strategy Alkali reduction again
Waste water and a large amount of body refuses for generating act on " secondary pollution " that environment generates, by the body refuse that can only be filled or burn change give up into
Treasured becomes industrial reusable raw material, creates certain economic benefit.On the one hand can be simple with whole set process, the TA of recycling
Grain size is big, and purity is high, can utilize again, on the other hand can reduce the processing load of remaining waste water, solves that processing cost is high to ask
Topic, environmental benefit and economic benefit are taken into account, while improving treatment effeciency, reduce environmental pollution.
Specific embodiment
Embodiment 1：The aluminium chloride for accounting for wastewater quality 20% is added in waste water, quickly stirs, adjusts the pH value of waste water
It to 11, mixes slowly, then through waste coal slag filtering precipitate, clear liquid is adsorbed through active carbon layer, then is filtered through one layer of waste coal slag blanket.It is past
In clear liquid be added account for wastewater quality 1% 800 mesh of mistake sieve terephthalic acid powder, after be slowly added to diluted acid, wait for clear liquid pH
After value is down to 3,15min is stood, for gained solid-liquid mixture by filter press press filtration, filter residue is washed, drying.
The acid value of product, total heavy metal content, coloration are according to SH/T 1612.1-2005《Industrial pure terephthalic acid》
It is detected, gained terephthalic acid (TPA) acid value is 668mgKOH/g, and total heavy metal content is 11mg/kg, coloration 10mg/kg.
By spectra methods, it is 99.3% to measure gained terephthalic acid (TPA) purity, and grain size is average at 53 μm.Water is milky white before filtering
Color crosses the transparent clarification of water after filter, and wastewater COD removal rate is 78.5% after filtering.
Embodiment 2：Be added in waste water and account for the aluminium chloride of wastewater quality 5%, quickly stirred, adjust the pH value of waste water to
10, it mixes slowly, then through waste coal slag filtering precipitate, clear liquid is adsorbed through active carbon layer, then is filtered through one layer of waste coal slag blanket.Toward clearly
In liquid be added account for wastewater quality 0.05% 500 mesh of mistake sieve terephthalic acid powder, after be slowly added to diluted acid, wait for clear liquid pH
After value is down to 2,15min is stood, for gained solid-liquid mixture by filter press press filtration, filter residue is washed, drying.
The acid value of product, total heavy metal content, coloration are according to SH/T 1612.1-2005《Industrial pure terephthalic acid》
It is detected, gained terephthalic acid (TPA) acid value is 668mgKOH/g, and total heavy metal content is 11.2mg/kg, coloration 10mg/
kg.By spectra methods, it is 99.1% to measure gained terephthalic acid (TPA) purity, and grain size is average at 51 μm.Water is breast before filtering
White crosses the transparent clarification of water after filter, and wastewater COD removal rate is 78.8% after filtering.
Embodiment 3：The aluminium chloride for accounting for wastewater quality 20% is added in waste water, quickly stirs, adjusts the pH value of waste water
It to 11, mixes slowly, then through waste coal slag filtering precipitate, clear liquid is adsorbed through active carbon layer, then is filtered through one layer of waste coal slag blanket.
Diluted acid is added, after clear liquid pH value is down to 2, stands 15min, for gained solid-liquid mixture by filter press press filtration, filter residue is washed,
Drying.
The acid value of product, total heavy metal content, coloration are according to SH/T 1612.1-2005《Industrial pure terephthalic acid》
It is detected, gained terephthalic acid (TPA) acid value is 665mgKOH/g, and total heavy metal content is 13.8mg/kg, coloration 11.3mg/
kg.By spectra methods, it is 98.6% to measure gained terephthalic acid (TPA) purity, and grain size is average at 10.8 μm.Water is before filtering
Milky is crossed water after filter and is not clarified, there is milky turbidity, and wastewater COD removal rate is 71.3% after filtering,.
Embodiment 4：The pH value of waste water is adjusted to 11, the aluminium chloride for accounting for wastewater quality 20% is added, quickly stirs, slowly
Speed stirring, then through waste coal slag filtering precipitate, clear liquid is adsorbed through active carbon layer, then filtered through one layer of waste coal slag blanket.Diluted acid is added,
After clear liquid pH value is down to 2,15min is stood, for gained solid-liquid mixture by filter press press filtration, filter residue is washed, drying.
The acid value of product, total heavy metal content, coloration are according to SH/T 1612.1-2005《Industrial pure terephthalic acid》
It is detected, gained terephthalic acid (TPA) acid value is 656mgKOH/g, and total heavy metal content is 14.5mg/kg, coloration 11.8mg/
kg.By spectra methods, it is 95.6% to measure gained terephthalic acid (TPA) purity, and grain size is average at 11.5 μm.Water is before filtering
Milky is crossed water after filter and is not clarified, there is milky turbidity, and wastewater COD removal rate is 72.9% after filtering.
The terephthalic acid powder of 500 mesh sieve was added it can be seen from embodiment, improves terephthalic acid (TPA) in waste water
The crystallite dimension of later stage particle, the crystal grain for being become larger, convenient for processes such as later stage filterings, and since terephthalic acid (TPA) grain size increases,
Better crystallinity degree, so purity accordingly improves.
It is enlightenment with above-mentioned desirable embodiment according to the present invention, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to determine its technical scope according to right.
Claims (1)
1. a kind of method obtaining bulky grain terephthalic acid crystals from alkali decrement waste water, which is characterized in that including walking as follows
Suddenly：
Step 1: the aluminium chloride for accounting for wastewater quality 5%~20% is added in waste water, quickly stirs, adjust the pH value of waste water
It to 10~11, mixes slowly, then through waste coal slag filtering precipitate, clear liquid is adsorbed through active carbon layer, then through one layer of waste coal slag blanket mistake
Filter；
Step 2: the terephthalic acid (TPA) of 500 mesh of the mistake sieve or 800 mesh sieve that account for wastewater quality 0.05%~1% is added into clear liquid
Powder is then slowly added to diluted acid, after clear liquid pH value is down to 2~3, stands 15min, gained solid-liquid mixture passes through filter press
Press filtration, filter residue is washed, drying；Gained terephthalic acid particles are big, and convenient for filtering, purity is recyclable sharp again up to 99% or more
With.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| TWI708761B (en) * | 2019-09-26 | 2020-11-01 | 遠東新世紀股份有限公司 | Method for manufacturing terephthalic acid |
| CN112499637A (en) * | 2020-12-31 | 2021-03-16 | 常州市五洲化工有限公司 | Method for preparing ultra-dispersed white carbon black by recycling alkali-reduction wastewater resources |
| CN112499666A (en) * | 2020-12-31 | 2021-03-16 | 常州市五洲化工有限公司 | Method for preparing high-dispersion zinc oxide by recycling alkali-reduced wastewater |
| CN112875749A (en) * | 2021-02-25 | 2021-06-01 | 江苏爱特恩高分子材料有限公司 | Method for preparing high-dispersion titanium dioxide by recycling alkali-reduced wastewater |
| CN112919684A (en) * | 2021-03-01 | 2021-06-08 | 江苏爱特恩高分子材料有限公司 | Method for preparing ultra-dispersed titanium dioxide by recycling alkali-reduction wastewater resources |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257064A (en) * | 1999-12-16 | 2000-06-21 | 陈定良 | Process for recovering terephthalic acid from alkali reduced sewage |
| CN103173845A (en) * | 2012-01-12 | 2013-06-26 | 江苏爱特恩高分子材料有限公司 | Production method and application of terephthalic metal slat whisker |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS60163843A (en) * | 1984-02-06 | 1985-08-26 | Mitsubishi Chem Ind Ltd | Method of recovery of terephthalic acid |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1257064A (en) * | 1999-12-16 | 2000-06-21 | 陈定良 | Process for recovering terephthalic acid from alkali reduced sewage |
| CN103173845A (en) * | 2012-01-12 | 2013-06-26 | 江苏爱特恩高分子材料有限公司 | Production method and application of terephthalic metal slat whisker |
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