CN107434765A - A kind of method of industrialized production di-butyl nylonic acid ester - Google Patents
A kind of method of industrialized production di-butyl nylonic acid ester Download PDFInfo
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- CN107434765A CN107434765A CN201610356122.3A CN201610356122A CN107434765A CN 107434765 A CN107434765 A CN 107434765A CN 201610356122 A CN201610356122 A CN 201610356122A CN 107434765 A CN107434765 A CN 107434765A
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- acid ester
- acid
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- butanol
- butyl
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Abstract
Industrialized production di-butyl nylonic acid ester method, material quality ratio are nylon acid:Adsorbent:N-butanol:Catalyst=1:0.01:1.12~1.2:0.009~0.015, step:Nylon acid, the n-butanol of total amount 20% are thrown into dissolution kettle, is warming up to 60 DEG C of formation mixed liquors;Adsorbent is added in the mixed liquor after dissolving and stirred 1 hour, is filtered;Mixed liquor after remaining n-butanol and filtering and catalyst are added in esterifying kettle, are warming up to 110~180 DEG C;Reaction 12 hours, stops when acid number is in 15~35mgKOH/g;Open vacuum to remove unreacted n-butanol, kettle temperature is risen to 160~190 DEG C, opens vacuum, di-butyl nylonic acid ester is separated with catalyst;The soda ash solution of equivalent and thick di-butyl nylonic acid ester are squeezed into, is stirred 20 40 minutes at a temperature of 60~70 DEG C;Stratification, release following water layer;Crude product after alkali cleaning is added in rectifying still, is warming up to 170~190 DEG C, moisture and impurity are sloughed by rectifying column;Open vacuum, from rectifying column lateral line discharging collect 190~230 DEG C between cut be product.
Description
Technical field
The present invention relates to the synthetic method of dibasic acid ester, and in particular to a kind of side of industrialized production di-butyl nylonic acid ester
Method.
Technical background
The conventional coalescents of acrylic emulsion are alcohol ester 12 at present, and the boiling point of alcohol ester 12 is 247 DEG C.However as European Union
Raising of the country to the requirement of water paint VOC emission, the boiling point of alcohol ester 12 can not meet market to Diamond Search water paint
It is required that.Therefore market in urgent need wants a kind of waterborne film-forming auxiliary agent of net taste Diamond Search to substitute alcohol ester 12.Di-butyl nylonic acid ester is exactly
A kind of aqueous acrylic emulsion coalescents of excellent net taste Diamond Search.With following characteristic:1. improve the film forming of emulsion paint
Can be used for many emulsion polymers of emulsion paint at normal temperatures can not complete film forming, and most be unable to film forming at low temperature.Breast
Shellac varnish must rely on coalescents to help film forming.Coalescents are typically to evaporate very slow solvent, such as all kinds of alcohol ethers, alcohol ether vinegar
Acid esters and ester alcohol etc..Their collective effect is softening lotion polymer particle, is merged them.Good film forming helps
Agent need to generally meet following condition:Good hydrolytic stability;Low freezing point;Moderate volatility;Efficient coalescence efficiency;
Low water solubility.Di-butyl nylonic acid ester coalescents are a kind of fabulous coalescents for emulsion paint.Except making breast
The MFT of shellac varnish reduce it is outer, di-butyl nylonic acid ester coalescents can also improve paint film weatherability, washable property, can
Color developing of spatter property, touch-up paint and improvement coating etc..The net taste and VOC effect ratio tradition of di-butyl nylonic acid ester simultaneously
Coalescents alcohol ester 12, alcohol ester 16 it is more advantageous.2. di-butyl nylonic acid ester coalescents can be in wider temperature and wet
The consistent of emulsion paint color is kept in the range of degree.Under normal circumstances, it is not easy film forming when film is dried at low temperature or film forming is bad,
Compared with the coating of normal film forming at normal temperatures, film coated surface can it is coarse, matt, even have cracking.For light emulsion paint
For, coarse surface will cause stronger light scattering, therefore the colour brightness of emulsion paint can become poor.In other words, not
The surface color brightness of synthermal lower coating is different.Di-butyl nylonic acid ester coalescents can make emulsion paint in low temperature and normal temperature
Under obtain the homogeneous good filming of gloss.In addition, addition di-butyl nylonic acid ester coalescents can improve pigment in emulsion paint
Uniformity and stability improvement emulsion paint color developing.3. after adding di-butyl nylonic acid ester, improve between resin particle
Coalescence, so as to reduce permeability of the coating to vapor;Coating dries the stress pine between binder resin caused by after-contraction
Relaxation improves tack of the coating to ground;The even closer combination of micelle, coating machinery intensity improves, so that film can
Resisting fractre and it is completely exfoliated, improves weatherability.
On the method reaction time of synthetic nylon acid di-n-butyl at present, yield is low, while product content does not reach
99.0%, and acid number is high, smell weight, can not meet the requirement of net taste.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of reaction time is short, high conversion rate, accessory substance
Less, catalyst amount is few and the synthetic method of the di-butyl nylonic acid ester of net taste.
Realize the technical scheme of above-mentioned purpose:
A kind of method of industrialized production di-butyl nylonic acid ester, raw material are nylon with catalyst and its dosage mass ratio
Acid:Adsorbent:N-butanol:Catalyst=1:0.01:1.12~1.2:0.009~0.015, comprise the following steps:1) nylon is thrown
Acid, the n-butanol of total amount 20% enter in dissolution kettle, are warming up to 60 DEG C of formation mixed liquors;2) after hypersober being added into dissolving
Mixed liquor in stir 1 hour, the mechanical admixtures such as adsorbent are got rid of by filter;3) by residue 80% n-butanol and
Mixed liquor and catalyst after filtering are added in esterifying kettle, are started to warm up, and kettle temperature need to be controlled at 110~180 DEG C;4) react
Sampling detection acid number, stops reaction when acid number is in 15~35mgKOH/g after 12 hours;5) vacuum is opened by unreacted n-butanol
Removing, rises to 160~190 DEG C by kettle temperature, opens vacuum, di-butyl nylonic acid ester is separated with catalyst;6) the pure of equivalent is squeezed into
Aqueous slkali and thick di-butyl nylonic acid ester, stir 20-40 minutes at a temperature of 60~70 DEG C;7) stratification, following water is released
Layer;8) crude product after alkali cleaning is added in rectifying still, is warming up to 170~190 DEG C, moisture and impurity are sloughed by rectifying column;9)
Open vacuum, from rectifying column lateral line discharging collect 190~230 DEG C between cut be product.
In a kind of preferable technical scheme, adsorbent is bentonite, diatomite, kaolin, activated carbon.By to having a competition
Test using diatomite as optimum absorbent.
In a kind of preferable technical scheme:Using solid acid as catalyst, solid acid is phosphotungstic acid, p-methyl benzenesulfonic acid, sulphur
Sour hydrogen sodium.It is preferred that phosphotungstic acid.
In a kind of preferable technical scheme, lactate synthesis product is separated catalyst with product by distillation mode,
Catalyst after separation is stayed in kettle, reusable when next time feeds intake.
In a kind of preferable technical scheme, carboxylate distillation is carried out under vacuum -0.095~-0.097Mpa, is esterified
Thing rectifying is carried out under vacuum -0.096~-0.098Mpa.
In a kind of preferable technical scheme, alkali cleaning is carried out with the sodium carbonate liquor that mass percentage concentration is 15~20%.
In a kind of preferable technical scheme, 1) rectifying column select efficient stainless steel wire corrugated wire gauze packing, and top is using arranging
Flowed back in pipe;2) rectifying column takes two lines to discharge, i.e., tower top water outlet and alcohol, side line go out di-butyl nylonic acid ester;3) tower after rectifying
Next time, which feeds intake, after the raffinate recovery of kettle reuses;4) bed stuffing height is 10 meters, and overall rectifying tower height degree is 15 meters.
In a kind of preferable technical scheme:When carrying out rectifying, first flowed back with 100~200L/H flow, until positive fourth
Alcohol and other organic impurities take off, and start to receive diisobutyl ester of nylon acids continuous discharge.
Using above-mentioned technical proposal, the method for di-butyl nylonic acid ester produced by the invention has the advantages that:
Normal pressing operation, control condition is gentle, is easy to industrialize;Coordinate between each step closely, it is cost-effective, beneficial to environmental protection;
Product acid number is low, high income, net taste.
Embodiment
The present invention is occurred esterification under catalyst action by nylon acid and n-butanol and is made, and reaction equation is such as
Under:
Using diatomite as optimum absorbent, vanadic anhydride and cupric oxide and polyphosphazene polymer in nylon acid are got rid of
Compound.Acid can be used to be used as catalyst, such as solid super-strong acid, be catalyst preferably with phosphotungstic acid.Mixing after esterification
, it is necessary to remove unreacted acidic materials with alkali cleaning after alcohol in thing is distilled out of, the preferential sodium carbonate liquor for using 15%-20%
As soda-wash solution.
Illustrate the present invention with embodiment below, but embodiment does not form any limitation of the invention.
Embodiment 1
Raw material and dosage:8100 kilograms of nylon acid, 9100 kilograms of n-butanol, 80 kilograms of phosphotungstic acid, 81 kilograms of diatomite.
Production stage:8100 kilograms of nylon acid is thrown, 1820 kilograms of n-butanol enters in dissolution kettle, is warming up to 60 DEG C.Throw silicon
81 kilograms of diatomaceous earth enters in dissolution kettle, stirs 1 hour, is separated the impurity such as diatomite with mixed liquor by filter.After separation
Mixed liquor enter in esterifying kettle, while add 7280 kilograms of 80 kilograms of phosphotungstic acid and n-butanol.Start to warm up, be esterified.
Temperature in the kettle can be raised steadily, and temperature control is at 110~180 DEG C.After reaction 12 hours, the sampling detection acid number from esterifying kettle,
Stop reaction when acid number reaches 15~35mgKOH/g.Open vacuum and deviate from unreacted n-butanol, kettle temperature is risen to 190 DEG C, very
Reciprocal of duty cycle is controlled in -0.095~-0.097Mpa, and di-butyl nylonic acid ester will just be steamed out into the separation realized with catalyst.It is residual in kettle
Liquid uses when feeding intake next time.The soda ash solution concentration for squeezing into equivalent is 15% and thick di-butyl nylonic acid ester, at 60~70 DEG C
At a temperature of stir 20-40 minutes, stratification, release following water layer.Crude product after alkali cleaning is added in rectifying still, is warming up to
170~190 DEG C, moisture and impurity are sloughed by rectifying column.Open vacuum system, vacuum degree control in -0.096~-0.098Mpa,
From rectifying column lateral line discharging collect 190~230 DEG C between cut be product.Next time is added to after kettle raffinate is collected in rectifying still
Recycled in esterifying kettle.
Rectifying column selects efficient stainless steel wire corrugated wire gauze packing, and top is flowed back using in tubulation;Rectifying column takes two lines to go out
Material, i.e., tower top water outlet and alcohol, side line go out di-butyl nylonic acid ester;Next time, which feeds intake, after the raffinate of tower reactor reclaims after rectifying reuses;
Bed stuffing height is 10 meters, and overall rectifying tower height degree is 15 meters.When carrying out rectifying, first flowed back with 100~200L/H flow, directly
Taken off to n-butanol and other organic impurities, start to receive diisobutyl ester of nylon acids continuous discharge.
The quality measurements of gained di-butyl nylonic acid ester:
Sequence number | Detection project | Index | Testing result |
1 | Outward appearance | Colourless transparent liquid | Colourless transparent liquid |
2 | Content (GC) % | ≥99.0 | 99.74 |
3 | Moisture content (ppm) | ≤1000 | 320 |
4 | Acid number (mgKOH/g) | ≤0.1 | 0.024 |
Embodiment 2
Raw material and dosage:8100 kilograms of nylon acid, 9100 kilograms of n-butanol, 80 kilograms of phosphotungstic acid, 81 kilograms of diatomite, essence
Evaporate kettle 200 kilograms of raffinate of recovery.
Production stage:8100 kilograms of nylon acid is thrown, 1820 kilograms of n-butanol enters in dissolution kettle, is warming up to 60 DEG C.Throw silicon
81 kilograms of diatomaceous earth enters in dissolution kettle, stirs 1 hour, is separated the impurity such as diatomite with mixed liquor by filter.After separation
Mixed liquor enter in esterifying kettle, while it is public to add 80 kilograms of phosphotungstic acid, 7280 kilograms of n-butanol and rectifying still recovery raffinate 200
Jin.Start to warm up, be esterified.Temperature in the kettle can be raised steadily, and temperature control is at 110~180 DEG C.After reaction 12 hours, from
Sampling detection acid number, stops reaction when acid number reaches 15~20mgKOH/g in esterifying kettle.Open vacuum and deviate from unreacted positive fourth
Alcohol, kettle temperature is risen to 190 DEG C, di-butyl nylonic acid ester is just steamed out realization in -0.095~-0.097Mpa by vacuum degree control
With the separation of catalyst.Raffinate uses when feeding intake next time in kettle.The soda ash solution concentration for squeezing into equivalent is 15% and thick nylon
Sour di-n-butyl, 20-40 minutes are stirred at a temperature of 60~70 DEG C, stratification, release following water layer.By the crude product after alkali cleaning
It is added in rectifying still, is warming up to 170~190 DEG C, moisture and impurity is sloughed by rectifying column.Open vacuum system, vacuum degree control
In -0.096~-0.098Mpa, from rectifying column lateral line discharging collect 190~230 DEG C between cut be product.Kettle is residual in rectifying still
Next time, which is added in esterifying kettle, after liquid is collected recycles.
Rectifying column selects efficient stainless steel wire corrugated wire gauze packing, and top is flowed back using in tubulation;Rectifying column takes two lines to go out
Material, i.e., tower top water outlet and alcohol, side line go out di-butyl nylonic acid ester;Next time, which feeds intake, after the raffinate of tower reactor reclaims after rectifying reuses;
Bed stuffing height is 10 meters, and overall rectifying tower height degree is 15 meters.When carrying out rectifying, first flowed back with 100~200L/H flow, directly
Taken off to n-butanol and other organic impurities, start to receive diisobutyl ester of nylon acids continuous discharge.
The quality measurements of gained di-butyl nylonic acid ester:
Sequence number | Detection project | Index | Testing result |
1 | Outward appearance | Colourless transparent liquid | Colourless transparent liquid |
2 | Content (GC) % | ≥99.0 | 99.81 |
3 | Moisture content (ppm) | ≤1000 | 361 |
4 | Acid number (mgKOH/g) | ≤0.1 | 0.019 |
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, make specific be altered or varied and belong to protection scope of the present invention.
Claims (9)
- A kind of 1. method of industrialized production di-butyl nylonic acid ester, it is characterised in that:Raw material and catalyst and its dosage quality Than for nylon acid:Adsorbent:N-butanol:Catalyst=1:0.01:1.12~1.2:0.009~0.015, comprise the following steps:1) throwing nylon acid, the n-butanol of total amount 20% enter in dissolution kettle, are warming up to 60 DEG C of formation mixed liquors;2) hypersober is added in the mixed liquor after dissolving and stirred 1 hour, it is by filter that the machinery such as adsorbent is miscellaneous Matter is got rid of;3) mixed liquor after the n-butanol of residue 80% and filtering and catalyst are added in esterifying kettle, started to warm up, kettle Temperature need to be controlled at 110~180 DEG C;4) sampling detection acid number, stops reaction when acid number is in 15~35mgKOH/g after reacting 12 hours;5) open vacuum to remove unreacted n-butanol, kettle temperature is risen to 160~190 DEG C, opens vacuum, by di-butyl nylonic acid ester Separated with catalyst;6) soda ash solution of equivalent and thick di-butyl nylonic acid ester are squeezed into, 20-40 minutes are stirred at a temperature of 60~70 DEG C;7) stratification, following water layer is released;8) crude product after alkali cleaning is added in rectifying still, is warming up to 170~190 DEG C, moisture and impurity are sloughed by rectifying column;9) open vacuum, from rectifying column lateral line discharging collect 190~230 DEG C between cut be product.
- 2. the method for industrialized production di-butyl nylonic acid ester according to claim 1, it is characterised in that:The adsorbent For bentonite, diatomite, kaolin or activated carbon.
- 3. the method for industrialized production di-butyl nylonic acid ester according to claim 1, it is characterised in that:The catalyst For solid acid.
- 4. the method for industrialized production di-butyl nylonic acid ester according to claim 3, it is characterised in that:The solid acid For phosphotungstic acid, p-methyl benzenesulfonic acid or niter cake.
- 5. the method for industrialized production di-butyl nylonic acid ester according to claim 1, it is characterised in that:By lactate synthesis Product is separated catalyst with product by distillation mode, and the catalyst after separation is stayed in kettle, and being repeated when next time feeds intake makes With.
- 6. the method for industrialized production di-butyl nylonic acid ester according to claim 1, it is characterised in that:Carboxylate distills Carried out under vacuum -0.095~-0.097Mpa, carboxylate rectifying is carried out under vacuum -0.096~-0.098Mpa.
- 7. the method for industrialized production di-butyl nylonic acid ester according to claim 1, it is characterised in that:With quality percentage The sodium carbonate liquor of concentration 15~20% carries out alkali cleaning.
- 8. the method for industrialized production di-butyl nylonic acid ester according to claim 1, it is characterised in that:1) rectifying column selects efficient stainless steel wire corrugated wire gauze packing, and top is flowed back using in tubulation;2) rectifying column takes two lines to discharge, i.e., tower top water outlet and alcohol, side line go out di-butyl nylonic acid ester;3) next time, which feeds intake, after the raffinate of tower reactor reclaims after rectifying reuses.4) bed stuffing height is 10 meters, and overall rectifying tower height degree is 15 meters.
- 9. the method for industrialized production di-butyl nylonic acid ester according to claim 1, it is characterised in that:Carry out rectifying When, first flowed back with 100~200L/H flow, until n-butanol and other organic impurities take off, start to receive nylon acid two Isobutyl ester continuous discharge.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108129316A (en) * | 2017-12-25 | 2018-06-08 | 江苏雷蒙新材料有限公司 | A kind of nylon acid two(2- ethyls)The preparation method of own ester |
CN108191649A (en) * | 2017-12-25 | 2018-06-22 | 江苏雷蒙新材料有限公司 | A kind of preparation method of dibutylester nylon acids |
CN113045414A (en) * | 2021-03-18 | 2021-06-29 | 润泰新材料股份有限公司 | Production process of dimethyl nylon acid |
CN115353454A (en) * | 2022-08-19 | 2022-11-18 | 润泰化学(泰兴)有限公司 | Preparation method of bio-based film-forming additive |
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CN113045414A (en) * | 2021-03-18 | 2021-06-29 | 润泰新材料股份有限公司 | Production process of dimethyl nylon acid |
CN115353454A (en) * | 2022-08-19 | 2022-11-18 | 润泰化学(泰兴)有限公司 | Preparation method of bio-based film-forming additive |
CN115353454B (en) * | 2022-08-19 | 2023-10-31 | 润泰化学(泰兴)有限公司 | Preparation method of bio-based film forming auxiliary agent |
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