CN104710300B - A kind of method extracting p-phthalic acid from terephthalic acid residue - Google Patents
A kind of method extracting p-phthalic acid from terephthalic acid residue Download PDFInfo
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- CN104710300B CN104710300B CN201510093797.9A CN201510093797A CN104710300B CN 104710300 B CN104710300 B CN 104710300B CN 201510093797 A CN201510093797 A CN 201510093797A CN 104710300 B CN104710300 B CN 104710300B
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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
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
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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
- C07C51/50—Use of additives, e.g. for stabilisation
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- Oil, Petroleum & Natural Gas (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The present invention relates to a kind of from the method extracting p-phthalic acid from terephthalic acid residue。Useless p-phthalic acid pulverizer is pulverized, puts in a small amount of water, form solid-liquid suspension, add sodium hydroxide solution and dissolve to particle。It is charged with the mixture of ferric chloride and polyacrylamide again, float is filtered。Trimethyl dihydroquinoline polymer powder is added in wherein, add dilute hydrochloric acid, and filter pressing will be precipitated with pressure filter。Gained precipitate is dried then through washing with acetone。The method utilizes useless p-phthalic acid as raw material, purifies the p-phthalic acid purity obtained up to 99.5%。Making it can be again with, environmental benefit and economic benefit be taken into account, and improve product utilization efficiency simultaneously, reduce environmental pollution。
Description
Technical field
The present invention relates to a kind of method extracting p-phthalic acid from terephthalic acid residue。
Background technology
P-phthalic acid is the dicarboxylic acids that yield is maximum in the world at present, it is mainly used in forming polyethylene terephthalate with ethylene glycol polycondensation, have another name called terylene, be widely used in and the various aspects of the national economy such as chemical fibre, light industry, electronics, building, live closely related with people。At present, refining p-phthalic acid main source is to be prepared by the catalyzed oxidation of xylol。
In textile printing and dyeing process process, Alkali reduction technology is widely used at present, and containing a large amount of para-phthalic sodiums in its waste water。Current textile printing and dyeing company is precipitated out mainly by acid out technology, but the useless terephthalic acid residue purity obtained is low, it is impossible to for industrial use, cause the wasting of resources。If being carried out purification, resource can be made effectively to be recycled。
Technology contents
The purpose of the present invention is exactly the method for purification proposing a kind of useless p-phthalic acid, improves the utilization rate of product。
It is an object of the present invention to obtain the method making p-phthalic acid can become good regenerated resources, the method utilizes useless p-phthalic acid as raw material, purifies the p-phthalic acid purity obtained up to 99.5%。
The invention provides a kind of method extracting p-phthalic acid from terephthalic acid residue, comprise the steps:
Step one, useless p-phthalic acid pulverizer is pulverized, particle size is below 100 μm, put in a small amount of water, form the solid-liquid suspension of solid content 50%～90%, stir under 300 revs/min, adding concentration in this suspension is the sodium hydroxide solution of 10mol/L～60mol/L, dissolves to particle；
Step 2, in the solution of step one, add the mixture of ferric chloride and polyacrylamide that mass ratio is 1:1～1:5, be stirring 3min under 1000 revs/min at rotating speed, after to transfer rotating speed to be stirring 5min under 200 revs/min, float is filtered；
Step 3, trimethyl dihydroquinoline polymer is crushed to more than 100 orders, add in step 2 gained supernatant liquid, stir under 300 revs/min, forming solid content is the solid-liquid suspension of 0.1%～5%, adding concentration is the hydrochloric acid solution of 10mol/L～50mol/L, form precipitation, filter pressing will be precipitated with pressure filter；
Step 4, gained precipitation is dried after, with washing with acetone 2～3 times, again dry。Gained p-phthalic acid purity is up to more than 99.5%。
The solution have the advantages that and efficiently solve " secondary pollution " effect that environment is produced by the useless p-phthalic acid of materializing strategy, the body refuse that can only fill or burn is turned waste into wealth, becomes industrial reusable raw material, create certain economic benefit。Make useless terephthaldehyde's acid starting material of recovery again with, environmental benefit and economic benefit are taken into account, and improve product utilization efficiency simultaneously, reduce environmental pollution。
Specific embodiment
Embodiment 1: being pulverized by useless p-phthalic acid pulverizer, particle size, at 100 μm, is put in a small amount of water, form the solid-liquid suspension of solid content 50%, stirring under 300 revs/min, adding concentration in this suspension is the sodium hydroxide solution of 10mol/L, dissolves to particle。In solution, add the mixture of ferric chloride and polyacrylamide that mass ratio is 1:1, be stirring 3min under 1000 revs/min at rotating speed, after to transfer rotating speed to be stirring 5min under 200 revs/min, float is filtered to obtain clear liquor。Trimethyl dihydroquinoline polymer being crushed to 100 orders, adds in gained supernatant liquid, stir under 300 revs/min, form the solid-liquid suspension that solid content is 0.1%, adding concentration is the hydrochloric acid solution of 10mol/L, forms precipitation, will precipitate filter pressing with pressure filter。After gained precipitation is dried, with washing with acetone 2 times, again dry。
The acid number of product, total heavy metal content, colourity detect according to SH/T1612.1-2005 " industrial pure terephthalic acid ", and gained p-phthalic acid acid number is 675mgKOH/g, and total heavy metal content is 9mg/kg, and colourity is 10mg/kg。By spectra methods, recording gained p-phthalic acid purity is 99.5%。
Embodiment 2: being pulverized by useless p-phthalic acid pulverizer, particle size, at 200 μm, is put in a small amount of water, form the solid-liquid suspension of solid content 90%, stirring under 300 revs/min, adding concentration in this suspension is the sodium hydroxide solution of 10mol/L, dissolves to particle。In solution, add the mixture of ferric chloride and polyacrylamide that mass ratio is 1:5, be stirring 3min under 1000 revs/min at rotating speed, after to transfer rotating speed to be stirring 5min under 200 revs/min, float is filtered to obtain clear liquor。Trimethyl dihydroquinoline polymer being crushed to 100 orders, adds in gained supernatant liquid, stir under 300 revs/min, form the solid-liquid suspension that solid content is 1%, adding concentration is the hydrochloric acid solution of 50mol/L, forms precipitation, will precipitate filter pressing with pressure filter。After gained precipitation is dried, with washing with acetone 3 times, again dry。
The acid number of product, total heavy metal content, colourity detect according to SH/T1612.1-2005 " industrial pure terephthalic acid ", and gained p-phthalic acid acid number is 675mgKOH/g, and total heavy metal content is 9mg/kg, and colourity is 9.5mg/kg。By spectra methods, recording gained p-phthalic acid purity is 99.6%。
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not necessarily departing from this invention technological thought, can carry out various change and amendment completely。The technical scope of this invention is not limited to the content in description, it is necessary to determine its technical scope according to right。
Claims (1)
1. the method extracting p-phthalic acid from terephthalic acid residue, comprises the steps:
Step one, useless p-phthalic acid pulverizer is pulverized, particle size is below 100 μm, put in a small amount of water, form the solid-liquid suspension of solid content 50%～90%, stir under 300 revs/min, adding concentration in this suspension is the sodium hydroxide solution of 10mol/L～60mol/L, dissolves to particle；
Step 2, in the solution of step one, add the mixture of ferric chloride and polyacrylamide that mass ratio is 1:1～1:5, be stirring 3min under 1000 revs/min at rotating speed, after to transfer rotating speed to be stirring 5min under 200 revs/min, float is filtered；
Step 3, trimethyl dihydroquinoline polymer is crushed to more than 100 orders, add in step 2 gained supernatant liquid, stir under 300 revs/min, forming solid content is the solid-liquid suspension of 0.1%～5%, adding concentration is the hydrochloric acid solution of 10mol/L～50mol/L, form precipitation, filter pressing will be precipitated with pressure filter；
Step 4, gained precipitation is dried after, with washing with acetone 2～3 times, again dry。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510093797.9A CN104710300B (en) | 2015-03-03 | 2015-03-03 | A kind of method extracting p-phthalic acid from terephthalic acid residue |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510093797.9A CN104710300B (en) | 2015-03-03 | 2015-03-03 | A kind of method extracting p-phthalic acid from terephthalic acid residue |
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| CN104710300A CN104710300A (en) | 2015-06-17 |
| CN104710300B true CN104710300B (en) | 2016-06-22 |
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| 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 |
| CN103922926A (en) * | 2014-04-17 | 2014-07-16 | 绍兴县远程树脂科技有限公司 | Process for purifying residual solid waste generated after alkali peeling wastewater treatment |
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Effective date of registration: 20160512 Address after: 213164 Jiangsu province Changzhou city Wujin District, Dong Po No. 10 Applicant after: Changzhou Wuyang Auxiliary Co., Ltd Address before: 213164 B, building 3, building No. 801, middle Wu Road, Wujin District, Jiangsu, Changzhou, China 10F Applicant before: Changzhou Bo Yang novel material Science and Technology Ltd. |
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Address after: 213164 Jiangsu province Changzhou city Wujin District, Dong Po No. 10 Patentee after: Changzhou Wuzhou Environmental Protection Technology Co., Ltd. Address before: 213164 Jiangsu province Changzhou city Wujin District, Dong Po No. 10 Patentee before: Changzhou Wuyang Auxiliary Co., Ltd |
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