CN106588638A - Method of purifying pure terephthalic acid (PTA) by means of white mud after treatment of textile alkali dissolution waste water and crude terephthalic acid after degradation of waste Dacron silk cloth - Google Patents
Method of purifying pure terephthalic acid (PTA) by means of white mud after treatment of textile alkali dissolution waste water and crude terephthalic acid after degradation of waste Dacron silk cloth Download PDFInfo
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- CN106588638A CN106588638A CN201611059709.4A CN201611059709A CN106588638A CN 106588638 A CN106588638 A CN 106588638A CN 201611059709 A CN201611059709 A CN 201611059709A CN 106588638 A CN106588638 A CN 106588638A
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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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- 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
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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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Abstract
The invention discloses a method of purifying pure terephthalic acid (PTA) by means of white mud after treatment of textile alkali dissolution waste water and crude terephthalic acid after degradation of waste Dacron silk cloth. The method includes the steps of: 1) integration of material addition, slurry blending and pre-heating: adding industrial reclaimed water or fresh industrial water accounting for 75-80% of total weight of raw materials into a slurry blending kettle, starting stirring and successively adding raw materials as well as high temperature activated carbon, a descaling agent, and a composite finishing additive, and feeding high-temperature reclaimed vapor after pressure reduced crystallization or temperature reduced crystallization to dissolve the raw materials and heat the raw materials to 150-180 DEG C to prepare slurry; 2) starting a tubular heater to heat the raw materials, and performing high-temperature and high-pressure filtration, pressure reduced crystallization, cooling and dehydration; and 3) wastewater treatment: neutralizing wastewater by lime, flocculating and discoloring the wastewater by a water purifying agent, and filtering the wastewater to remove residues, so that the purified industrial water can be applied in the material addition and slurry blending step. The method accelerates dissolution and filtration and saves energy cost and changes production from intermittent type into continuous type, thus improving production efficiency. The method has beneficial to balance of production processes, and reduces man-hour cost.
Description
Technical field
The present invention relates to technical field of chemical purification, more particularly, to the white clay after being processed with weaving alkali soluble technique waste water and
The method of thick PTA purified terephthalics after the waste and old silk cloth degraded of terylene.
Background technology
P-phthalic acid（PTA）A kind of important Organic Chemicals, be mainly used for produce polyester fiber (terylene),
Mylar and polyester bottles, are widely used in the national economy various aspects such as chemical fibre, light industry, electronics, building, with people's lives
The height of level is closely related.In the application of PTA, more than 90% PTA is used to produce polyethylene terephthalate in the world
Ester (PET), other parts are as PTT（PTT）And polybutylene terephthalate (PBT)（PBT）And
The raw material of other products.
According to customs statistics, since nineteen ninety, China PTA import volume is in rapid growth trend year by year, from nineteen ninety-five extremely
Between 15 years in 2010, average growth rate per annum reaches 22.07%, wherein especially most fast to increase between 2000 to 2006 years, average growth rate per annum
Up to 44.26%.It is expected that China PTA production capacity in 2016 is up to 9,430,000 t, demand is up to 13,000,000 t.Estimated 2016
Year whole world PTA production capacity and consumption figure reach 40,000,000 t, and production and consumption is in a basic balance.
As p-phthalic acid is in the industry life such as polyester, fiber, plasticizer thermosetting alkyd resin, unsaturated polyester resin
Extensive application in product, the commercial production total amount of PTA rapidly increase.Although to its production technology constantly improve and improvement, every year
Still there are the PTA white clays of hundred million ton of weaving alkali soluble wastewater treatments up to a hundred to be handled.As a variety of causes contains in the sewage of discharge
The PTA having after substantial amounts of weaving alkali soluble wastewater treatment, is deposited into sludge-like white clay because PTA is water insoluble, PTA contents in white clay
Up to 80～90%, there is the white clay ton up to a million brought because of PTA productions not obtain effective resource reclaim and utilize every year, it is existing
The method for processing the PTA white clays of this weaving alkali soluble wastewater treatment is to burn, and in waste material, 90% or so useful composition is not played
Its due use value.The PTA white clays of domestic weaving alkali soluble wastewater treatment are more accumulated the more, the PTA of alkali soluble wastewater treatment of weaving
White clay is classified as the resource of reproducible utilization by national environmental protection portion, and the PTA white clays for how dealing carefully with weaving alkali soluble wastewater treatment are
The current difficult problem that manufacturing enterprise faces both at home and abroad.Therefore effectively solving PTA waste recovery processing method is found, can be both made full use of
PTA waste materials, reduce PTA production costs, can reduce the pollution to environment again, and this is that current PTA manufacturing enterprises are imminent needs
The problem of solution.
In current PTA waste recovery processing methods, the country mostly takes three kinds of methods：
Water vapour sublimed method：The characteristic for being easy to distil using benzoic acid derivative, PTA waste materials are used at superheated vapour
Reason, benzoic acid derivative are reached and are separated with pure mixed phthalic acid with water vapor stream is steamed；
Esterified by butyl alcohol method：By PTA waste materials and esterified by butyl alcohol, Jing vacuum distillations obtain mixing butyl benzoate and benzene mixed two
Formic acid dibutyl ester, then hydrolysis are separated out, and butanol is recyclable.
Methanol esterification method：Technological process is similar to esterified by butyl alcohol method, is esterified with waste material with methanol, and fractional distillation is mixed
Essence of Niobe and pure mixed phthalic acid dimethyl ester.
The external comprehensive utilization to PTA waste materials is mainly used to waste material by following several approach：
P-phthalic acid is directly reclaimed from waste material, first the residual acid in waste material is neutralized with alkali so as to be converted into water solublity gold
Category salt, is heated to 300～380 DEG C in atmosphere after drying, oxidation a few hours are soluble in water salt while hot, acidified to be returned
The p-phthalic acid of receipts.
P -carboxybenzaldehyde is extracted from waste material, is heated together with PTA waste materials with propanol, toluene and toluene sulfonic acide
Which is reacted l hours at 50 DEG C with hydrochloric acid, is obtained by backflow, then two propanol of al of Jing separated available 87% together
98.2% p -carboxybenzaldehyde.In this reaction, the conversion ratio of two propanol of al is 100%, and this method can be carried well
Go out the higher p -carboxybenzaldehyde of purity so as to further apply in other industry.
The comprehensive utilization of PTA waste materials.The PTA waste materials of pie or pasty state are mutually mixed with petroleum oil, water phase is removed
Afterwards, then with another appropriate petroleum oil mutually mix, a kind of fuel oil is obtained；After PTA being purified, remaining waste material exists
Acetic acid is sloughed under the conditions of 220 DEG C/0.1MPa, Jing after air oxidation 0.5～2 hour, is steamed under the conditions of 140～180 DEG C/4-8KPa
Evaporate, the mixture of highly purified p-methylbenzoic acid and phthalic acid be just obtained, the ratio of the molal quantity of the two is 4 ~ 19: l,
This mixture can be used to the products such as production paint, preservative.
The each have their own advantage of above processing method and deficiency, but above-mentioned these methods all adopt and size mixing, preheat and entered with kettle
Row dissolving, blood pressure lowering crystallization and dewatered drying basic technology, mostly there are vapourss consumption greatly, and long the production cycle and production are not
Problem in a balanced way.
And for PTA production leftover bits and pieces and the waste and old silk cloth of terylene currently mostly by mound bury or incinerating method at
Reason, thus the waste of waste materials is not only caused, while can also cause environmental pollution, destroy ecological balance.
The content of the invention
For the problem deposited in above-mentioned existing purification terephthalic acid process's technology, the invention provides a kind of not only give birth to
Produce cycle is short, produce sustainable balance；In production process, steam and industrial water circulation comprehensive are utilized, and can reduce the energy and water again
Resource consumption, the method for reducing production cost.This technique refining effect is good, and purification purity is high, can effectively remove terephthaldehyde
Float in acid salt solution, the terephthalate product purity after refining is up to more than 98%.This technique both adapts to weaving alkali soluble and gives up
White clay after water process adapts to the thick PTA purified terephthalics after the waste and old silk cloth degraded of terylene again.
The thick PTA purifications after the waste and old silk cloth degraded of white clay and terylene after the alkali soluble wastewater treatment with weaving of the present invention are right
The method of phthalic acid is：
（1）Feed intake, size mixing, it is pre- heating integrated：Be initially charged in kettle of sizing mixing the 75-80% of raw material gross weight industrial reuse water or
Fresh process water, opens stirring, then high temperature active charcoal, raw material gross weight 0.5- for putting into raw material gross weight 4-6 ‰ successively
1.5% scale remover and the composite finishing auxiliary agent of raw material gross weight 2-3 ‰, the composite finishing auxiliary agent is by anion surface active
Agent LAS, AES and nonionic surfactant AEO mix composition by weight for LAS: AES: AEO=5: 3: 2, then put into meter
Measured raw material, the raw material include white clay, thick PTA, the high temperature reuse steam after being passed through blood pressure lowering crystallization or decrease temperature crystalline, by original
Material dissolves and is warming up to 150-180 DEG C makes slurry, and controls slurry solid content for 15～20%, then defeated by high-temperature high pressure pump
Dissolve in delivering to pipeline heater；
（2）Tubular type dissolves：Tube heater heating, then opening conduits formula heater charging and discharging valve are opened, opening high-pressure pump will be upper
Slurry input tube heater dissolving is stated, flow is adjusted, dissolution velocity is controlled according to yield, solution outlet pipe temperature should reach after dissolving
To 260-300 DEG C, pressure is 5.5-6.0MPa；
（3）High Temperature High Pressure is filtered：The solution that pipeline heater has dissolved is put into metallic conduit formula filter carries out high temperature, height
Press filtration, temperature 250-280 DEG C, pressure 5.4-5.8MPa filter insoluble debris；
（4）Blood pressure lowering is crystallized：Again by step（3）Obtained filtrate is put into crystallization kettle, after first crystallization kettle solution is piled, opens
Second crystallization kettle, turns off first crystallization kettle, after solution is filled in crystallization kettle, turns off inlet valve, open steam valve blood pressure lowering knot
It is brilliant；Just started in kettle pressure high, the steam of discharge be put into feed intake, preheat, integrated kettle of sizing mixing, when in crystallization kettle, pressure is
Turn off exhaust steam valve during 0.6Mpa, prepare discharge, while the inlet valve being also switched off on integrated kettle；
（5）Cooling, dehydration：Material after blood pressure lowering is crystallized enters decrease temperature crystalline kettle decrease temperature crystalline and is cooled to 40-50 DEG C, while will
Waste heat during decrease temperature crystalline lead to all the way feed intake, preheat, integrated kettle of sizing mixing, another road lead to tray drying bed be dried produce
Product；Material after cooling is dehydrated by screen cloth vibration, when material moisture is 1-2%, is transferred to the drying of tray drying bed；
（6）Drying, packaging：Material after dehydration is transported to into tray drying bed, is dried to material moisture and is less than 0.5%, pack,
Enter storehouse；
（7）Sewage disposal：Neutralize through Calx, after water purification agent flocculation decoloration, after filter cleaner, the industry water after purification is used further to
Feed intake and size mixing.
The technique effect of the present invention：
1st, the present invention will feed intake, size mixing heating integrated with pre-, and comprehensively utilize the used heat that blood pressure lowering crystallization and cooled dehydrated discharge and steam
Vapour；
Heat for sizing mixing and preheating, often process 1 ton of PTA waste material and can save 0.3 ton of steam consumption, by 65 yuan/ton of steam cost
Calculate, the processing meanss of 50,000 tons of PTA of a set of annual output, only can save ten thousand yuan of 50000 × 0.3 × 65=97.5 by steam cost every year；
2nd, duct type electrothermal device continuous-dissolution was changed to kettle and steam heating for dissolving originally, High Temperature High Pressure pipe was adopted after dissolving
Road formula filter is filtered, and is accelerated dissolving and the rate of filtration, is saved energy cost, make production be changed to continuous way by batch (-type),
Production efficiency is improve, and is conducive to balancing between production process, reduce work time cost；
3rd, the present invention can be used for weaving the white clay purification processes after alkali soluble wastewater treatment, can be used for silk cloth drop waste and old from terylene again
The purified terephthalics such as the thick PTA after solution, improve equipment efficiency of usage；
4th, the PTA purity purified by the present invention can reach more than 98%.
P-phthalic acid specific targets
The present invention adds a small amount of high temperature active charcoal when sizing mixing, and for the decolouring and degumming of serosity, is additionally added a small amount of scale remover
With composite finishing auxiliary agent, soften and improve the mobility of serosity for water for industrial use.
The present invention is refined to benzene using the thick PTA after the waste and old silk cloth degraded of white clay and terylene after weaving alkali soluble wastewater treatment
Dioctyl phthalate, the PTA white clays after alkali soluble wastewater treatment of weaving are classified as the resource of renewable comprehensive utilization, middle international politics by national environmental protection portion
Mansion exists《Textile industry " 12 " development plan》Explicitly point out accelerate to the policy guide of waste textile recycling and
Fund input,《Planning》In especially emphasize " minimizing, recycling, resource " theory, meet national recycling economy industrial policy,
Project implementation has good economic benefit, environmental benefit and social benefit.
Description of the drawings：
Fig. 1 is the process chart of the present invention,
Fig. 2 is pipeline heater combining structure schematic diagram,
Fig. 3 is the structural representation of pipeline heater.
Specific embodiment:
It is as shown in Figure 1 in process chart, in Refining Terephthalic Acid, white after the alkali soluble wastewater treatment with weaving
Thick PTA after mud and the waste and old silk cloth degraded of terylene purifies the method for p-phthalic acid：
（1）Feed intake, size mixing, it is pre- heating integrated：The industrial reuse water of the 75-80% of raw material weight or new is added in kettle of sizing mixing first
Fresh water for industrial use, opens stirring, then puts into high temperature active charcoal successively（For 5/1000ths of raw material weight）, scale remover（Raw material weight
One of percentage of amount）With composite finishing auxiliary agent（For raw material weight thousand/bis- point five）, the composite finishing auxiliary agent by the moon from
Sub- surfactant LAS, AES and nonionic surfactant AEO are LAS: AES: AEO=5: 3: 2 by weight）Mixing and
Into, finally put into the white clay or/and thick PTA raw materials for measuring, the high temperature reuse steam after being passed through blood pressure lowering crystallization or decrease temperature crystalline,
By material dissolution and be warming up to 150-180 DEG C and make slurry, and slurry solid content is controlled for 15～20%, then by High Temperature High Pressure
Pump is dissolved in being delivered to pipeline heater；
（2）Tubular type dissolves：Pipeline heater heating, then opening conduits heater charging and discharging valve are opened, opening high-pressure pump will be upper
The dissolving of slurry input channel formula heater is stated, flow is regulated, dissolution velocity, solution outlet pipe after control dissolving are controlled according to yield
Temperature should reach more than 260-300 DEG C, pressure 5.5-6.0MPa；
（3）High Temperature High Pressure is filtered：The solution that tube heater has been dissolved carries out high temperature, height by metal tube filter and presses through
Filter, temperature 250-270 DEG C, pressure 5.4-5.8MPa filter insoluble debris；
（4）Blood pressure lowering is crystallized：Again will be through step（3）Filtrate after high temperature, high-pressure metal tubular filter are filtered is put into crystallization kettle,
After first crystallization kettle solution is piled, second crystallization kettle is opened, turns off first crystallization kettle, when solution is filled in crystallization kettle
Afterwards, turn off inlet valve, open steam valve blood pressure lowering crystallization has just started pressure height in kettle, and the steam of discharge is put into and feeds intake, preheats, sizing mixing
Integrated kettle, turns off exhaust steam valve when pressure is 0.6MPa in crystallization kettle, prepares discharge, while being also switched off entering on integrated kettle
Steam valve；
（5）Cooling and dehydration：The further decrease temperature crystalline of material after blood pressure lowering is crystallized is cooled to 40-50 DEG C, while cooling is tied
Residual heat integrative during crystalline substance is utilized, lead to all the way feed intake, preheat, integrated kettle of sizing mixing, another road is led to tray drying bed and is entered
Row drying.Material after cooling is dehydrated by screen cloth vibration, when material moisture is 1-2%, is transferred on tray drying bed and is done
It is dry；Simultaneously the water of abjection is circulated for sizing mixing Jing after process is up to standard；
（6）Drying and packaging：Material after dehydration is transported to into tray drying bed, is dried to material moisture and is less than 0.5%, packaging
Enter storehouse；
(7) sewage disposal：Neutralize through Calx, water purification agent flocculation decoloration, filter cleaner, the industry water after purification is used further to throw
Material is sized mixing.
The pipeline heater structure（As shown in Figures 2 and 3）It is including the earthenware 9 that head and the tail are connected with intervalve 10, described
First earthenware carries last root earthenware with a last liquid outlet 2, on liquid outlet with a beginning inlet 1
Liquid temp detector 3 is provided with out, temperature measurer 4 in electrothermal tube and pipe in earthenware, is provided with, electrothermal tube is by connection jaws 5 and electricity
Source is connected, and protective cover 6 is provided with connection jaws, and earthenware support 7 is supported, and deflector 8 is arranged at intervals with the electrothermal tube.
Claims (1)
1. the refined terephthaldehydes of thick PTA after the white clay and the waste and old silk cloth of terylene after a kind of alkali soluble wastewater treatment using weaving is degraded
The method of acid, its feature will be in：Methods described step is：
（1）Feed intake, size mixing, it is pre- heating integrated：Be initially charged in kettle of sizing mixing the 75-80% of raw material gross weight industrial reuse water or
Fresh process water, opens stirring, then high temperature active charcoal, raw material gross weight 0.5- for putting into raw material gross weight 4-6 ‰ successively
1.5% scale remover and the composite finishing auxiliary agent of raw material gross weight 2-3 ‰, the composite finishing auxiliary agent is by anion surface active
Agent LAS, AES and nonionic surfactant AEO are mixed for LAS: AES: AEO=5: 3: 2 by weight, then put into meter
Measured raw material, the raw material include white clay, thick PTA, the high temperature reuse steam after being passed through blood pressure lowering crystallization or decrease temperature crystalline, by original
Material dissolves and is warming up to 150-180 DEG C makes slurry, and controls slurry solid content for 15～20%, then defeated by high-temperature high pressure pump
Dissolve in delivering to pipeline heater；
（2）Tubular type dissolves：Tube heater heating, then opening conduits heater charging and discharging valve are opened, opening high-pressure pump will be above-mentioned
Slurry input tube heater dissolving, adjusts flow, controls dissolution velocity according to yield, and after control dissolving, solution outlet pipe temperature should
260 DEG C ~ 300 DEG C are reached, pressure 5.5-6.0MPa；
（3）High Temperature High Pressure is filtered：The solution that pipeline heater has been dissolved carries out high temperature, high pressure by metal tube filter
Filter, 250 ~ 270 DEG C of temperature, pressure 5.4-5.8MPa filter insoluble debris；
（4）Blood pressure lowering is crystallized：Again by step（3）Obtained filtrate is put into crystallization kettle, after first crystallization kettle solution is piled, opens
2nd crystallization kettle, turns off first crystallization kettle；After solution is filled in crystallization kettle, turn off inlet valve, open steam valve blood pressure lowering knot
Crystalline substance, it is high just to have started in kettle pressure, the steam of discharge be put into feed intake, preheat, integrated kettle of sizing mixing, when in crystallization kettle, pressure is
Turn off exhaust steam valve during 0.6MPa, prepare discharge, while the inlet valve being also switched off on integrated kettle；
（5）Cooling and dehydration：The further fully decrease temperature crystalline of material after blood pressure lowering is crystallized, is cooled to 40-50 DEG C, while will drop
Waste heat in warm crystallization process lead to all the way feed intake, preheat, integrated kettle of sizing mixing, another road lead to tray drying bed be dried produce
Product, the material after cooling are dehydrated by screen cloth vibration, when material moisture is 1-2%, are transferred to drying on tray drying bed；
Simultaneously the water of abjection is circulated for sizing mixing Jing after process is up to standard；
（6）Drying and packaging：Material after dehydration is transported to into tray drying bed, is dried to material moisture and is less than 0.5%, packaging
Enter storehouse；
(7) sewage disposal：Neutralize through Calx, water purification agent flocculation decoloration, filter cleaner, the industry water after purification is used further to throw
Material is sized mixing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611059709.4A CN106588638B (en) | 2016-11-28 | 2016-11-28 | A method of with the white clay after weaving alkali soluble wastewater treatment and the thick PTA purified terephthalic after the waste and old silk cloth degradation of terylene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611059709.4A CN106588638B (en) | 2016-11-28 | 2016-11-28 | A method of with the white clay after weaving alkali soluble wastewater treatment and the thick PTA purified terephthalic after the waste and old silk cloth degradation of terylene |
Publications (2)
| Publication Number | Publication Date |
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| CN106588638A true CN106588638A (en) | 2017-04-26 |
| CN106588638B CN106588638B (en) | 2018-12-07 |
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| CN201611059709.4A Active CN106588638B (en) | 2016-11-28 | 2016-11-28 | A method of with the white clay after weaving alkali soluble wastewater treatment and the thick PTA purified terephthalic after the waste and old silk cloth degradation of terylene |
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| CN103408421A (en) * | 2013-08-21 | 2013-11-27 | 深圳市超纯环保股份有限公司 | Terephthalic acid purification method |
| CN105873890A (en) * | 2013-12-31 | 2016-08-17 | Bp北美公司 | Oxidation process for preparing purified carboxylic acids |
| CN105873892A (en) * | 2013-12-30 | 2016-08-17 | Bp北美公司 | Purification of aromatic carboxylic acids |
| CN106032351A (en) * | 2015-03-14 | 2016-10-19 | 王建中 | Crude PTA purification method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5481033A (en) * | 1994-12-22 | 1996-01-02 | E. I. Du Pont De Nemours And Company | Purification process for aromatic dicarboxylic acids |
| US20050228195A1 (en) * | 2004-04-09 | 2005-10-13 | Wytcherley Randi W | Purification of carboxylic acids by complexation with selective solvents |
| CN101001825A (en) * | 2004-04-09 | 2007-07-18 | Gtc技术公司 | Purification of carboxylic acids by complexation with selective solvents |
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| CN103408421A (en) * | 2013-08-21 | 2013-11-27 | 深圳市超纯环保股份有限公司 | Terephthalic acid purification method |
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| CN106032351A (en) * | 2015-03-14 | 2016-10-19 | 王建中 | Crude PTA purification method |
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| CN106588638B (en) | 2018-12-07 |
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