CN106966892A - A kind of purifying process of crude terephthalic acid - Google Patents
A kind of purifying process of crude terephthalic acid Download PDFInfo
- Publication number
- CN106966892A CN106966892A CN201710212397.4A CN201710212397A CN106966892A CN 106966892 A CN106966892 A CN 106966892A CN 201710212397 A CN201710212397 A CN 201710212397A CN 106966892 A CN106966892 A CN 106966892A
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- CN
- China
- Prior art keywords
- terephthalic acid
- crude terephthalic
- crude
- water
- pta
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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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
-
- 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
Abstract
The invention discloses a kind of purifying process of crude terephthalic acid, step（1）By the crude terephthalic acid reclaimed in dyeing waste water and water by 3:10 solid water ratios are sequentially added in dissolvers, are then stirred and are warming up to untill crude terephthalic acid is completely dissolved, are further continued for being heated to crude terephthalic acid for fritting melt body；Step（2）The crude terephthalic acid under filtering semi-molten state removes insoluble solid finely ground particles while hot；Step（3）Crude terephthalic acid under double of molten condition, which continues to add water to, to be completely dissolved, and then carries out quick refrigeration to less than 8 DEG C, crude terephthalic acid crystal is separated out, and centrifugal filtration isolates soluble impurity and obtains pure terephthalic acid (PTA) crystal；Step（4）Pure terephthalic acid (PTA) crystal is inserted in vacuum drying decomposer, kinetics obtain pure terephthalic acid (PTA).The present invention, which is separated off impurity, makes the high purity more than 98% of terephthalic acid (TPA), and the purification rate of terephthalic acid (TPA) is improved to the full extent, recycling is realized, actual operation requirements are met.
Description
Technical field
The present invention relates to a kind of purifying process of crude terephthalic acid, belong to alkali decrement waste water processing technology field.
Background technology
Terephthalic acid (TPA), also known as p- phthalic acids, are the maximum dicarboxylic acids of yield, are mainly made by paraxylene, are
Produce the primary raw material of polyester.It is solid under normal temperature, heats non-fusible, more than 300 DEG C distillations, if being heated in closed container,
Can be in 425 DEG C of fusings；Water is insoluble under normal temperature, mainly for the manufacture of synthesizing polyester resin, synthetic fibers and plasticizer etc..It is thick right
The method of purification of phthalic acid：Comprise the following steps, crude terephthalic acid is dried, ball milling, screening, particle diameter is reached 1~5 μ
M, at a temperature of 60 DEG C -100 DEG C, is impregnated in water, stirring, clarification and then slash water, finally centrifuges, 80 DEG C -105
DEG C drying, obtains pure terephthalic acid (PTA), described crude terephthalic acid is sediment of the alkali decrement waste water after acid out, impurity
Butt weight content is 15%-18%.
Alkali reduction is textile printing and dyeing enterprises to dacron at high temperature to terylene macromolecular ester linkage hydrolyzing, corrosion, is promoted
Fibr tissue relaxes, and mitigates fabric weight, so that fabric has a kind of new technology of silky touch.But, the production of Alkali reduction process
Given birth to organic spent lye of a large amount of high concentrations containing phenyl ring, COD is up to 6000-15000, its main component have para-phthalic sodium,
One of ethylene glycol etc., it is difficult to handle, primary pollution source as enterprise.This part of contaminated water is more intractable, if by waste liquid
Terephthalic acid (TPA) is reclaimed, and pollutional load can be not only greatly lowered（COD）, its terephthalic acid (TPA) is alternatively arranged as important having
Machine industrial chemicals is able to recycling.Domestic some enterprise implements terephthalic acid (TPA) recovery measure, makes COD significantly drop
It is low, but each enterprise's dyeing and printing process is different, alkali decrement waste water complicated components, pretreatment and acid out process unit imperfection, reclaims
It is thick small to dioctyl phthalate particle diameter（Generally 5-10um）Filtration difficulty, moisture content is big（More than 50%）, impurity height, it is difficult to be used as change
Work raw material is directly utilized, and waste resource influences environment again.For this reason, it may be necessary to a kind of new technical scheme is designed, can be comprehensive
Solve the deficiency that prior art is present.
The content of the invention
The present invention is separated exactly in view of the deficienciess of the prior art, provide a kind of purifying process of crude terephthalic acid
Removing impurity makes the high purity more than 98% of terephthalic acid (TPA), and the purification rate of terephthalic acid (TPA) is improved to the full extent, realizes
Recycling, meets actual operation requirements.
To solve the above problems, the technical solution used in the present invention is as follows：
A kind of purifying process of crude terephthalic acid, comprises the following steps：
Step（1）：By the crude terephthalic acid reclaimed in dyeing waste water and water by 3:10 solid water ratio is sequentially added in dissolvers
Dissolving, then stirs and uniformly heats up, untill crude terephthalic acid and water are completely dissolved, and is further continued for being heated to slightly to benzene two
Formic acid is fritting melt body；
Step（2）：The crude terephthalic acid filtered while hot under the semi-molten state of above-mentioned formation removes small of insoluble solid
Grain thing；
Step（3）：Crude terephthalic acid under above-mentioned semi-molten state is continued to add water until being completely dissolved, then to completely molten
Crude terephthalic acid under the semi-molten state of solution carries out quick refrigeration to less than -8 DEG C using circulating cooling system, slightly to benzene two
Formic acid crystal is separated out, and centrifugal filtration isolates soluble impurity and obtains pure terephthalic acid (PTA) crystal；
Step（4）：Pure terephthalic acid (PTA) crystal is inserted in vacuum drying decomposer, in the range of 180-260 DEG C, 3-5 hours,
Kinetics obtain pure terephthalic acid (PTA)（The high purity more than 99.2% of gained terephthalic acid (TPA)）.
As the improvement of above-mentioned technical proposal, in the step（1）In simultaneously also be added with activated carbon or bleaching earth adsorption agent
In a kind of decolorization adsorption impurity, and the adsorbent consumption be crude terephthalic acid 2-4%.
As the improvement of above-mentioned technical proposal, the circulating cooling system includes circulation cold flow room and the cooling used cooperatively
Room, the circulation cold flow outside wall be provided with airflow inlet, the circulation cold flow room be provided with cooling medium, air-introduced machine and
The condensation fiber tube used cooperatively；Matter Transfer import is provided with the cooling chamber.
Compared with prior art, implementation result of the invention is as follows by the present invention：
The feature for the wet crude terephthalic acid that the present invention is reclaimed for dyeing waste water, the principle crystallized using dissolving and quick refrigeration
It is combined, while eliminating the insoluble and water-solubility impurity contained in crude terephthalic acid, improves crystal grain and be beneficial to filtering behaviour
Make, improve the purity of crude terephthalic acid purifying process, reduce purifying cost, make the high purity of gained terephthalic acid (TPA)
More than 99.2%.
In addition, as important industrial chemicals, for the manufacture of plasticizer and coating resin, purification media is recyclable to be made
With the Optimum utilization of resource being realized, with good environmental benefit and economic benefit.
Brief description of the drawings
Fig. 1 is circulating cooling system structural representation of the present invention.
Embodiment
Illustrate present disclosure below in conjunction with specific embodiments.
Embodiment
As shown in figure 1, being a kind of purifying process of crude terephthalic acid described in the present embodiment, comprise the following steps：
Step（1）：By the crude terephthalic acid reclaimed in dyeing waste water and water by 3:10 solid water ratio is sequentially added in dissolvers
Dissolving, then stirs and uniformly heats up, untill crude terephthalic acid and water are completely dissolved, and is further continued for being heated to slightly to benzene two
Formic acid is fritting melt body；
Step（2）：The crude terephthalic acid filtered while hot under the semi-molten state of above-mentioned formation removes small of insoluble solid
Grain thing；
Step（3）：Crude terephthalic acid under above-mentioned semi-molten state is continued to add water until being completely dissolved, then to completely molten
Crude terephthalic acid under the semi-molten state of solution carries out quick refrigeration to less than -8 DEG C using circulating cooling system, slightly to benzene two
Formic acid crystal is separated out, and centrifugal filtration isolates soluble impurity and obtains pure terephthalic acid (PTA) crystal；
Step（4）：Pure terephthalic acid (PTA) crystal is inserted in vacuum drying decomposer, in the range of 180-260 DEG C, 3-5 hours,
Kinetics obtain pure terephthalic acid (PTA)（The high purity more than 99.2% of gained terephthalic acid (TPA)）.
Specifically, in step（1）In simultaneously also added with a kind of decolorization adsorption impurity in activated carbon or bleaching earth adsorption agent,
And the consumption of the adsorbent is the 2-4% of crude terephthalic acid.
More specifically, the circulating cooling system includes circulation cold flow room 10 and the cooling chamber 20 used cooperatively, it is described to follow
The lateral wall of ring cold flow room 10 is provided with airflow inlet 11, the circulation cold flow room 10 and is provided with cooling medium 12, air-introduced machine 13
And the condensation fiber tube 14 used cooperatively；Matter Transfer import 21 is provided with the cooling chamber 20.
The feature for the wet crude terephthalic acid that the present invention is reclaimed for dyeing waste water, is crystallized using dissolving and quick refrigeration
Principle is combined, while eliminating the insoluble and water-solubility impurity contained in crude terephthalic acid, is improved crystal grain and was beneficial to
Filter operation, improves the purity of crude terephthalic acid purifying process, reduces purifying cost, makes the purity of gained terephthalic acid (TPA)
Up to more than 99.2%.
Note：The terephthalic acid (TPA) is alternatively arranged as important industrial chemicals, for the manufacture of plasticizer and coating resin,
Purification media can be recycled, and realize the Optimum utilization of resource, with good environmental benefit and economic benefit.
Above content is made for the present invention in conjunction with specific embodiments describes in detail, it is impossible to assert that the present invention is specific real
Apply and be only limitted to these explanations.For those skilled in the art, before present inventive concept is not departed from
Put, some simple deduction or replace can also be made, the scope of protection of the invention should be all considered as belonging to.
Claims (3)
1. a kind of purifying process of crude terephthalic acid, it is characterised in that：Comprise the following steps：
Step（1）：By the crude terephthalic acid reclaimed in dyeing waste water and water by 3:10 solid water ratio is sequentially added in dissolvers
Dissolving, then stirs and uniformly heats up, untill crude terephthalic acid and water are completely dissolved, and is further continued for being heated to slightly to benzene two
Formic acid is fritting melt body；
Step（2）：The crude terephthalic acid filtered while hot under the semi-molten state of above-mentioned formation removes small of insoluble solid
Grain thing；
Step（3）：Crude terephthalic acid under above-mentioned semi-molten state is continued to add water until being completely dissolved, then to completely molten
Crude terephthalic acid under the semi-molten state of solution carries out quick refrigeration to less than -8 DEG C using circulating cooling system, slightly to benzene two
Formic acid crystal is separated out, and centrifugal filtration isolates soluble impurity and obtains pure terephthalic acid (PTA) crystal；
Step（4）：Pure terephthalic acid (PTA) crystal is inserted in vacuum drying decomposer, in the range of 180-260 DEG C, 3-5 hours,
Kinetics obtain pure terephthalic acid (PTA)（The high purity more than 99.2% of gained terephthalic acid (TPA)）.
2. a kind of purifying process of crude terephthalic acid according to claim 1, it is characterised in that：In the step（1）In
Simultaneously also added with a kind of decolorization adsorption impurity in activated carbon or bleaching earth adsorption agent, and the consumption of the adsorbent is slightly to benzene
The 2-4% of dioctyl phthalate.
3. a kind of purifying process of crude terephthalic acid according to claim 1, it is characterised in that：The circulating cooling system
Including circulation cold flow room（10）And the cooling chamber used cooperatively（20）, the circulation cold flow room（10）Lateral wall is provided with air-flow and entered
Mouthful（11）, the circulation cold flow room（10）Inside it is provided with cooling medium（12）, air-introduced machine（13）And the condensation fiber tube used cooperatively
（14）；The cooling chamber（20）On be provided with Matter Transfer import（21）.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710212397.4A CN106966892A (en) | 2017-04-01 | 2017-04-01 | A kind of purifying process of crude terephthalic acid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710212397.4A CN106966892A (en) | 2017-04-01 | 2017-04-01 | A kind of purifying process of crude terephthalic acid |
Publications (1)
| Publication Number | Publication Date |
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| CN106966892A true CN106966892A (en) | 2017-07-21 |
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ID=59336752
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710212397.4A Pending CN106966892A (en) | 2017-04-01 | 2017-04-01 | A kind of purifying process of crude terephthalic acid |
Country Status (1)
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121655A (en) * | 2007-08-30 | 2008-02-13 | 洪芳柏 | Technique for purifying crude terephthalic acid |
-
2017
- 2017-04-01 CN CN201710212397.4A patent/CN106966892A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121655A (en) * | 2007-08-30 | 2008-02-13 | 洪芳柏 | Technique for purifying crude terephthalic acid |
Non-Patent Citations (1)
| Title |
|---|
| 上海进出口商品检验局: "《进出口商品检验方法 化工原料及化工产品分册》", 31 August 1999, 上海科学普及出版社 * |
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Application publication date: 20170721 |