CN109809988A - A kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate - Google Patents
A kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate Download PDFInfo
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- CN109809988A CN109809988A CN201910232171.XA CN201910232171A CN109809988A CN 109809988 A CN109809988 A CN 109809988A CN 201910232171 A CN201910232171 A CN 201910232171A CN 109809988 A CN109809988 A CN 109809988A
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Abstract
The present invention relates to the production methods that a kind of PTA reclaimed materials is esterified preparation dioctyl terephthalate, belong to PTA reclaimed materials reutilization technology field.The present invention recycles PTA reclaimed materials, generates environment-friendlyplasticizer plasticizer dioctyl terephthalate, from technological design angle, feeding mode, temperature, in terms of optimize.Compared with prior art, advantageous effects of the present invention are that production link is energy-efficient, and catalyst is used multiple times, and isooctanol utilization rate is high；Shorten the reaction time, the reaction time controls in 12~16h.
Description
Technical field
The present invention relates to PTA reclaimed materials reutilization technology field, in particular to a kind of PTA reclaimed materials esterification preparation is to benzene two
The production method of formic acid dioctyl ester.
Background technique
PTA reclaimed materials refers to the pair containing a small amount of mechanical admixture that p-phthalic acid generates in production, transportational process
Product, but purity is very high, if irrational utilization, not only results in waste of resources, but also pollute the environment.From view of theory, PTA reclaimed materials
It can be used to produce the environment-friendly plasticizer DOTP plasticizer and have vast market prospect, so that it is bright that PTA reclaimed materials can be generated
Aobvious economic value.
Dioctyl terephthalate is a kind of primary plasticizer of function admirable of polyvinyl-chloride use.Its performance is the same as current city
Dioctyl phthalate performance on field is substantially suitable, the enhancing however as people to environmental consciousness, terephthalic acid (TPA)
Dioctyl ester as environment-friendlyplasticizer plasticizer one kind and be primary plasticizer, can gradually be largely used to each neck of polyvinyl chloride soft goods
Domain, dioctyl terephthalate also act as the increasing of synthetic rubber other than being largely used to the plasticizer of CABLE MATERIALS, polyvinyl chloride
Mould agent, coating additive, lubricant additive, it is also possible to make the softening agent of paper.
PTA and isooctanol reaction preparation dioctyl terephthalate, are first converted to mono octyl ester, and resterification is double monooctyl esters, is turned
The speed of chemical conversion mono octyl ester is much more slowly than the speed that resterification is double monooctyl esters, this directly affects PTA and prepares terephthalic acid (TPA) two
The speed of monooctyl ester.When handling PTA reclaimed materials, it is desirable to increase W-response speed.
Summary of the invention
The present invention provides the production methods that PTA reclaimed materials is esterified preparation dioctyl terephthalate, from technological design angle
Degree sets out, and solves above-mentioned technical problem.
The technical scheme is that a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate, packet
Include following steps:
S1, it quantitative isooctanol is directly pumped into after high-order measuring tank from raw alcohol tank puts into esterifying kettle, open stirring, stir
Mixing speed is 750~950r/min, PTA reclaimed materials spiral cast feeder is put into esterifying kettle, the process that feeds intake esterifying kettle is closed；It can
Reduce PTA reclaimed materials and the volatilization of isooctanol inorganization；
S2, the heating of conduction oil valve is opened after the completion of feeding intake, when alcohol-water separation tank has reflux and kettle temperature reaches 180 DEG C,
Esterifying kettle is added in catalyst butyl titanate by normal pressure, and butyl titanate dosage is 1 ‰~the 5 ‰ of PTA reclaimed materials quality,
The water generated in reaction process and excessive octanol form alcohol-water azeotrope, liquid phase are formed after condenser condenses, through alcohol moisture
Alcohol, water are separated from device, upper layer octanol passes back into esterifying kettle, and the reaction was continued, and lower layer generates water and is discharged into water pot, and conduction oil continues to heat,
Temperature≤230 DEG C, the reaction was continued when not changing to alcohol-water separation device liquid level, and being considered as reaction terminates；
S31, crude product mention alcohol, reduce esterifying kettle temperature, open vacuum pump and will mention alcohol kettle and vacuumize, and material sucking mentioned
Alcohol kettle mentions alcohol kettle temperature degree at 170 DEG C~230 DEG C first with sensible heat, recycling conduction oil control under vacuum conditions, will slightly produce
Isooctanol in product proposes that isooctanol is returned esterifying kettle after proposing the condensation of alcohol condenser and is recycled, the crude product after mentioning alcohol
It squeezes into and neutralizes kettle purification；
S32, mention crude product after alcohol import neutralize kettle after open conduction oil and control 90 DEG C of temperature of charge or so, and it is metered
Lye be stirred generation neutralization reaction, after the reaction was completed, kettle temperature rises to 170 DEG C, opens vacuum pump and will neutralize kettle system and takes out
Vacuum is passed through low-pressure steam into neutralization kettle at vacuum condition (- 0.1MPa), by the moisture contained in material and isooctanol band
Kettle is neutralized out, after condenser is cooling, separates alcohol, water through alcohol-water separation device, isooctanol continues to participate in anti-as raw material reuse
It answers；
S33, filtering kettle is poured into after material cools down, qualitative activity charcoal is added, be stirred a period of time, open filter pump
Material is squeezed into plate and frame filter press, filters out active carbon and floccule therein, filtrate enters daily output product after cooler cools down
Tank, as finished product dioctyl terephthalate.
Further, in S1, isooctanol: PTA is 2.4~3:1 (the ratio between amount of substance).In one embodiment, different
Octanol: PTA is 2.5:1 (the ratio between amount of substance), reaction time 12h.
Further, in S1, mixing speed 885r/min.
Further, butyl titanate dosage is the 3 ‰ of PTA reclaimed materials quality.
Further, in S32, the lye for neutralizing addition is KOH solution.
Be substantially carried out at 180 DEG C monoesters reaction, dibasic acid esters reaction carry out slowly, dibasic acid esters react required temperature condition be 210~
230℃.Isooctanol is first added in esterifying kettle, PTA reclaimed materials is added by spiral cast feeder, on the one hand, can under screw action
PTA reclaimed materials is refined, the specific surface area of PTA particle is increased；On the other hand, PTA reclaimed materials is to be gradually added into, and isooctanol is excessive；
Phase before the reaction can all accelerate the monoesters reaction speed of PTA, and then shorten the reaction time.Reaction time is in 12~16h.
Esterification is reversible reaction.In S2, by-product water is exported in time, while the ethylhexanol reflux taken out of returns ester
Change kettle to be reacted.It is carried out conducive to reaction to positive direction, improves reaction conversion ratio.
In technological design, in S2, S31 and S32, it can all flow in esterifying kettle, improve different again after isooctanol separation
The utilization rate of octanol saves the dosage of isooctanol.
The present invention recycles PTA reclaimed materials, generates environment-friendlyplasticizer plasticizer dioctyl terephthalate；With prior art phase
Than advantageous effects of the present invention are that production link is energy-efficient, and catalyst is used multiple times, and isooctanol utilization rate is high；Shorten
Reaction time, reaction time control in 12~16h.
Specific embodiment
The specific embodiment of the invention is described below with reference to embodiment:
A kind of embodiment 1: production method of PTA reclaimed materials esterification preparation dioctyl terephthalate, comprising the following steps:
S1, it 325g isooctanol is directly pumped into after high-order measuring tank from raw alcohol tank puts into esterifying kettle, open stirring, stirring
Speed is 885r/min, 166gPTA reclaimed materials spiral cast feeder is put into esterifying kettle, the process that feeds intake esterifying kettle is closed；
S2, the heating of conduction oil valve is opened after the completion of feeding intake, when alcohol-water separation tank has reflux and kettle temperature reaches 180 DEG C,
Esterifying kettle is added in 0.5g butyl titanate by normal pressure, and the water and excessive octanol generated in reaction process forms alcohol-water azeotrope,
Liquid phase is formed after condenser condenses, separates alcohol, water through alcohol-water separation device, upper layer octanol passes back into esterifying kettle, and the reaction was continued, under
Layer generates water and is discharged into water pot, and conduction oil continues to heat, temperature≤230 DEG C, and the reaction was continued does not become to alcohol-water separation device liquid level
When change, being considered as reaction terminates；
S31, crude product mention alcohol, reduce esterifying kettle temperature, open vacuum pump and will mention alcohol kettle and vacuumize, and material sucking mentioned
Alcohol kettle mentions alcohol kettle temperature degree at 170 DEG C~230 DEG C first with sensible heat, recycling conduction oil control under vacuum conditions, will slightly produce
Isooctanol in product proposes that isooctanol is returned esterifying kettle after proposing the condensation of alcohol condenser and is recycled, the crude product after mentioning alcohol
It squeezes into and neutralizes kettle purification；
S32, mention crude product after alcohol import neutralize kettle after open conduction oil and control 90 DEG C of temperature of charge or so, and it is metered
KOH solution be stirred generation neutralization reaction, after the reaction was completed, kettle temperature rises to 170 DEG C, and kettle system will be neutralized by opening vacuum pump
It vacuumizes, low-pressure steam is passed through into neutralization kettle at vacuum condition (- 0.1MPa), by the moisture contained in material and isooctanol
It takes neutralization kettle out of, after condenser is cooling, separates alcohol, water through alcohol-water separation device, isooctanol continues to participate in anti-as raw material reuse
It answers；
S33, filtering kettle is poured into after material cools down, qualitative activity charcoal is added, be stirred a period of time, open filter pump
Material is squeezed into plate and frame filter press, filters out active carbon and floccule therein, filtrate enters daily output product after cooler cools down
Tank, as finished product dioctyl terephthalate.
The yield of dioctyl terephthalate reaches 98.6%, purity 99%；Reaction time is 12.5h.
A kind of embodiment 2: production method of PTA reclaimed materials esterification preparation dioctyl terephthalate, comprising the following steps:
S1, it 312g isooctanol is directly pumped into after high-order measuring tank from raw alcohol tank puts into esterifying kettle, open stirring, stirring
Speed is 950r/min, 166gPTA reclaimed materials spiral cast feeder is put into esterifying kettle, the process that feeds intake esterifying kettle is closed；
S2, the heating of conduction oil valve is opened after the completion of feeding intake, when alcohol-water separation tank has reflux and kettle temperature reaches 180 DEG C,
Esterifying kettle is added in 0.8g butyl titanate by normal pressure, and the water and excessive octanol generated in reaction process forms alcohol-water azeotrope,
Liquid phase is formed after condenser condenses, separates alcohol, water through alcohol-water separation device, upper layer octanol passes back into esterifying kettle, and the reaction was continued, under
Layer generates water and is discharged into water pot, and conduction oil continues to heat, temperature≤230 DEG C, and the reaction was continued does not become to alcohol-water separation device liquid level
When change, being considered as reaction terminates；
S31, crude product mention alcohol, reduce esterifying kettle temperature, open vacuum pump and will mention alcohol kettle and vacuumize, and material sucking mentioned
Alcohol kettle mentions alcohol kettle temperature degree at 170 DEG C~230 DEG C first with sensible heat, recycling conduction oil control under vacuum conditions, will slightly produce
Isooctanol in product proposes that isooctanol is returned esterifying kettle after proposing the condensation of alcohol condenser and is recycled, the crude product after mentioning alcohol
It squeezes into and neutralizes kettle purification；
S32, mention crude product after alcohol import neutralize kettle after open conduction oil and control 90 DEG C of temperature of charge or so, and it is metered
KOH solution be stirred generation neutralization reaction, after the reaction was completed, kettle temperature rises to 170 DEG C, and kettle system will be neutralized by opening vacuum pump
It vacuumizes, low-pressure steam is passed through into neutralization kettle at vacuum condition (- 0.1MPa), by the moisture contained in material and isooctanol
It takes neutralization kettle out of, after condenser is cooling, separates alcohol, water through alcohol-water separation device, isooctanol continues to participate in anti-as raw material reuse
It answers；
S33, filtering kettle is poured into after material cools down, qualitative activity charcoal is added, be stirred a period of time, open filter pump
Material is squeezed into plate and frame filter press, filters out active carbon and floccule therein, filtrate enters daily output product after cooler cools down
Tank, as finished product dioctyl terephthalate.
The yield of dioctyl terephthalate reaches 96.3%, purity 99%；Reaction time is 15h.
Embodiment 3:
A kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate, comprising the following steps:
S1, it 390g isooctanol is directly pumped into after high-order measuring tank from raw alcohol tank puts into esterifying kettle, open stirring, stirring
Speed is 750r/min, 166gPTA reclaimed materials spiral cast feeder is put into esterifying kettle, the process that feeds intake esterifying kettle is closed；
S2, the heating of conduction oil valve is opened after the completion of feeding intake, when alcohol-water separation tank has reflux and kettle temperature reaches 180 DEG C,
Esterifying kettle is added in 0.2g butyl titanate by normal pressure, and the water and excessive octanol generated in reaction process forms alcohol-water azeotrope,
Liquid phase is formed after condenser condenses, separates alcohol, water through alcohol-water separation device, upper layer octanol passes back into esterifying kettle, and the reaction was continued, under
Layer generates water and is discharged into water pot, and conduction oil continues to heat, temperature≤230 DEG C, and the reaction was continued does not become to alcohol-water separation device liquid level
When change, being considered as reaction terminates；
S31, crude product mention alcohol, reduce esterifying kettle temperature, open vacuum pump and will mention alcohol kettle and vacuumize, and material sucking mentioned
Alcohol kettle mentions alcohol kettle temperature degree at 170 DEG C~230 DEG C first with sensible heat, recycling conduction oil control under vacuum conditions, will slightly produce
Isooctanol in product proposes that isooctanol is returned esterifying kettle after proposing the condensation of alcohol condenser and is recycled, the crude product after mentioning alcohol
It squeezes into and neutralizes kettle purification；
S32, mention crude product after alcohol import neutralize kettle after open conduction oil and control 90 DEG C of temperature of charge or so, and it is metered
KOH solution be stirred generation neutralization reaction, after the reaction was completed, kettle temperature rises to 170 DEG C, and kettle system will be neutralized by opening vacuum pump
It vacuumizes, low-pressure steam is passed through into neutralization kettle at vacuum condition (- 0.1MPa), by the moisture contained in material and isooctanol
It takes neutralization kettle out of, after condenser is cooling, separates alcohol, water through alcohol-water separation device, isooctanol continues to participate in anti-as raw material reuse
It answers；
S33, filtering kettle is poured into after material cools down, qualitative activity charcoal is added, be stirred a period of time, open filter pump
Material is squeezed into plate and frame filter press, filters out active carbon and floccule therein, filtrate enters daily output product after cooler cools down
Tank, as finished product dioctyl terephthalate.
The yield of dioctyl terephthalate reaches 99.1%, purity 99%；Reaction time is 16h.
Many other changes and remodeling can be made by not departing from the spirit and scope of the present invention.It should be appreciated that the present invention is not
It is limited to specific embodiment, the scope of the present invention is defined by the following claims.
Claims (7)
1. a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate, which is characterized in that
The following steps are included:
S1, it quantitative isooctanol is directly pumped into after high-order measuring tank from raw alcohol tank puts into esterifying kettle, open stirring, stirring speed
Degree is 750~950r/min, PTA reclaimed materials spiral cast feeder is put into esterifying kettle, the process that feeds intake esterifying kettle is closed；
S2, the heating of conduction oil valve is opened after the completion of feeding intake, when alcohol-water separation tank has reflux and kettle temperature reaches 180 DEG C, normal pressure,
Esterifying kettle is added in catalyst butyl titanate, butyl titanate dosage is 1 ‰~the 5 ‰ of PTA reclaimed materials quality, is reacted
The water generated in journey and excessive octanol form alcohol-water azeotrope, form liquid phase after condenser condenses, through alcohol-water separation device point
From alcohol, water, upper layer octanol passes back into esterifying kettle, and the reaction was continued, and lower layer generates water and is discharged into water pot, and conduction oil continues to heat, and temperature≤
230 DEG C, the reaction was continued when not changing to alcohol-water separation device liquid level, and being considered as reaction terminates；
Material needs in S3, esterifying kettle are further processed, and by mentioning the refining steps such as alcohol, neutralization, stripping, decoloration, can be made
Obtain environment-friendly plasticizer DOTP.
2. a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate according to claim 1, special
Sign is, S3 includes: that S31, crude product mention alcohol, reduces esterifying kettle temperature, opens vacuum pump and will mention alcohol kettle and vacuumizes, by material
Sucking mentions alcohol kettle, mentions alcohol kettle temperature degree at 170 DEG C~230 DEG C first with sensible heat, recycling conduction oil control under vacuum conditions, incites somebody to action
Isooctanol in crude product proposes that isooctanol is returned esterifying kettle after proposing the condensation of alcohol condenser and is recycled, thick after mentioning alcohol
Product, which is squeezed into, neutralizes kettle purification；
S32, mention crude product after alcohol import neutralize kettle after open conduction oil and control 90 DEG C of temperature of charge or so, with metered alkali
Liquid is stirred generation neutralization reaction, and after the reaction was completed, kettle temperature rises to 170 DEG C, opens vacuum pump and vacuumizes kettle system is neutralized,
At vacuum condition (- 0.1MPa) low-pressure steam is passed through to neutralizing in kettle, the moisture contained in material and isooctanol are taken out of
And kettle separates alcohol, water through alcohol-water separation device after condenser is cooling, isooctanol continues to participate in reaction as raw material reuse；
S33, filtering kettle is poured into after material cools down, qualitative activity charcoal is added, be stirred a period of time, open filter pump for object
Material squeezes into plate and frame filter press, filters out active carbon and floccule therein, and filtrate enters daily output products pot after cooler cools down, i.e.,
For finished product dioctyl terephthalate.
3. a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate according to claim 1, special
Sign is, in S1, isooctanol: PTA is 2.4~3:1 (the ratio between amount of substance).
4. a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate according to claim 1, special
Sign is, in S1, isooctanol: PTA is 2.5:1 (the ratio between amount of substance).
5. a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate according to claim 4, special
Sign is, in S1, mixing speed 885r/min.
6. a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate according to claim 1, special
Sign is, in S2, butyl titanate dosage is the 3 ‰ of PTA reclaimed materials quality.
7. a kind of production method of PTA reclaimed materials esterification preparation dioctyl terephthalate according to claim 2, S32
In, the lye for neutralizing addition is KOH solution.
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Cited By (2)
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| CN110642716A (en) * | 2019-11-13 | 2020-01-03 | 山东成武易信环保科技有限公司 | DOTP continuous distillation process |
| TWI719689B (en) * | 2019-10-28 | 2021-02-21 | 南亞塑膠工業股份有限公司 | Method for manufacturing and decolorizing dioctyl terephthalate |
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