CN108129316A - A kind of nylon acid two（2- ethyls）The preparation method of own ester - Google Patents
A kind of nylon acid two（2- ethyls）The preparation method of own ester Download PDFInfo
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- CN108129316A CN108129316A CN201711417379.6A CN201711417379A CN108129316A CN 108129316 A CN108129316 A CN 108129316A CN 201711417379 A CN201711417379 A CN 201711417379A CN 108129316 A CN108129316 A CN 108129316A
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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
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
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Abstract
The invention discloses a kind of nylon acids two（2 ethyls）The preparation method of own ester, belongs to chemical field.This method is that raw material passes through the series of processes such as dissolving, filtering, esterification, rectifying, alkali cleaning, washing, air lift, decoloration, dehydration, filtering using nylon acid, obtains the nylon acid two of high-quality（2 ethyls）Own ester product.Product index：Content >=99.0%, color and luster（Platinum cobalt colorimetric）≤ 30#, moisture≤0.10%, the mgKOH/g of acid value≤0.1.Simple production process of the present invention, raw material is cheap and easy to get, and yield is high, does not need to special reaction, isolates and purifies equipment, is very suitable for industrialized production, has very big economic benefit and social benefit.
Description
Technical field
It is reacted the present invention relates to one kind by industrial production adipic acid by-product leftover bits and pieces nylon acid with 2-Ethylhexyl Alcohol, prepares and close
Into mixed dibasic acid two（2- ethyls）The method of own ester, belongs to chemical field.
Background technology
Nylon acid also known as mixed dibasic acid, are the by-products of industrial production adipic acid, and main component is succinic acid, penta 2
Acid and adipic acid.
According to the production technology level of the current country, rough estimate, China's production adipic acid about has 50000 tons every year
Nylon acid generates.For efficiently using for nylon acid, country's mature technology, is primarily used to prepare nylon acid dimethyl ester at present,
It is with excellent chemistry, physical property：Boiling point is high, solvability is strong, toxicity is low, biodegradability is good, is a kind of novel
Environmentally friendly solvent, can be substituted in certain formulas isophorone, propylene glycol ether solvent use.There is patent（Publication number
CN1327975A）Report, using atmosphere intermission method prepare nylon acid dimethyl ester method, by nylon acid with methanol urging in strong acid
Under change effect through being esterified, slightly evaporating, alkali cleaning, the series of processes finished product such as rectifying.
Aliphatic dicarboxylic acid ester, such as dioctyl adipate（DOA）, dioctyl sebacate（DOS）, exist as plasticizer
In PVC product so that product of rubber and plastic has good low temperature cold tolerance, is a kind of excellent cold-resistant plasticizer, in recent years
Comparatively fast developed, demand rises year by year.There is a kind of patent " side using industrial by-products nylon acid production cold resistant plasticizer
Method "（Publication number CN103012128A, Feng Lie, Jiang Pingping）, method is using nylon acid and middle Long carbon chain alcohol（2- propyl enanthols）
Synthesize a kind of plasticizer under metatitanic acid ester catalysis, wherein raw material 2- propyl enanthols are a kind of novel plasticizer alcohol, this experiment people
The product color produced according to its method is deeper, darkly brown oil liquid, is unsatisfactory for the application of certain specific demands.
Invention content
The by-product leftover bits and pieces nylon acid of adipic acid and 2- ethyls are utilized in view of the deficiencies of the prior art, the present invention provides a kind of
Hexanol reacts, and prepares nylon acid two（2- ethyls）The preparation method of own ester can be applied to be used as a performance in product of rubber and plastic
Excellent cold-resistant plasticizer uses, and cold resistance is suitable with DOA, but cost but declines much, is a kind of novel environmental protection
Plasticizer, cost of implementation is low, high income, production safety, simple and practicable industrialized production, the nylon acid two of preparation（2- ethyls）
Own ester has many advantages, such as that acid value is low, content is high, lighter color.
Purpose to realize the present invention provides a kind of nylon acid two（2- ethyls）The preparation method of own ester, it is characterised in that with
The by-product leftover bits and pieces nylon acid of industrial production adipic acid is raw material and 2-Ethylhexyl Alcohol（It is commonly called as industrial octanol）Esterification occurs,
Prepare high-quality nylon acid two（2- ethyls）Own ester.Concrete operation step is as follows：
a）First nylon acid and 2-Ethylhexyl Alcohol are dissolved for 1: 2.1~1: 3.6 in dissolution kettle by the mass ratio that feeds intake, feed intake matter
Amount is than preferably 1: 2.4~1: 3.0.Solution temperature is controlled at 70~95 DEG C, and the material dissolved is filtered operation,
Remove the solid insoluble in nylon acid；After material reaches solution temperature in kettle, continue 0.5~1.0 h of stirring, to ensure material
Fully dissolving.
b）Material enters esterifying kettle, adds in 0.1 ‰~1 ‰ catalyst of material gross mass, preferably 0.4 ‰~0.6 ‰,
5~20% water entrainer of material gross mass, preferably 10~15%, specific dosage is determined according to the band outlet capacity of water entrainer, stirring
Heating starts esterification, and esterification temperature is controlled at 170~240 DEG C, and preferably esterification temperature is 185~230 DEG C；Esterification time
Control is 8~9 h in 6~10 h, preferably esterification time, separates the water that esterification generates in reaction process from water knockout drum in time,
Until there is no water generation, while sampling analysis, esterifying liquid acid value is surveyed, until during acid value≤1mgKOH/g, esterification reaches eventually
Point, you can stop reaction；
The present invention relates to the specific methods for adding in catalyst：Catalyst adds in two batches, after reflux is generated in esterifying kettle,
Catalyst can be added in, first amount added in is the 60~70% of catalyst total amount, after 5~6h of reaction, addition residue 30~
40% catalyst.
c）Material is transferred to dealcoholysis kettle, deviate under conditions of 0.094~0.096MPa of vacuum degree excessive 2-Ethylhexyl Alcohol and
Water entrainer, dealcoholysis temperature are 130~230 DEG C, and preferably dealcoholysis temperature is 150~210 DEG C, the 2-Ethylhexyl Alcohol and water entrainer of abjection
Esterifying kettle is returned to reuse；
d）The ester liquid that dealcoholysis terminates enters rectifying still, and 200~240 DEG C are collected under 0.096~0.098MPa of condition of high vacuum degree
Fraction obtains thick ester sample；Its color and luster（Platinum cobalt colorimetric number）In 50~60#, 0.8~1.2mgKOH/g of acid value, before 200 DEG C
The front-end volatiles steamed, return in dissolution kettle and reuse；Distillation operation is not evaporated, and distillation residual liquid, which is returned in dissolution kettle, to be repeated to make
With；
e）Thick ester sample enters alkali cleaning kettle, adds in lye, carries out alkali cleaning, and lye dosage is the thick ester production of 100~200kg lye/ton
Product, stratification, the ester liquid on upper strata enter washing kettle；Softened water is added in, the dosage of softened water is 200~300kg water/thick ester of ton
Product, most preferably, softening water consumption are the thick ester product of 250kg water/ton, are washed, stratification, the ester liquid on upper strata enters gas
Carry kettle；The operation temperature of alkali cleaning and water-washing step is controlled at 60~90 DEG C；Most preferably, the temperature of alkali cleaning is 60~70 DEG C.It is optimal
Choosing, the temperature of washing is 80~90 DEG C.In addition the lower water that water-washing step separates can be reused when preparing lye, be reduced
The discharge of sewage.
f）Upper strata ester liquid pump after washing is entered into air lift kettle, high-temperature vapor is slowly introducing in air lift bottom portion, in condition of high vacuum degree
Under the conditions of slough a small amount of 2-Ethylhexyl Alcohol and low-boiling-point substance present in ester liquid；The 2-Ethylhexyl Alcohol taken out of during air lift returns to molten
It is reused in solution kettle；The steam temperature used is 140 DEG C, and the dosage of vapor is 100~150kg/ tons of thick esters, during air lift
Between for 2~3h, air lift operation temperature is 150~160 DEG C, and vacuum degree is 0.096~0.098MPa；
g）Ester liquid pump after air lift is entered into refining kettle, decolorising agent of the dosage for 0.2~0.6kg/ tons of products is added in, in vacuum degree
It is carried out under 0.094~0.096MPa, temperature is 120~140 DEG C, carries out dehydration and decolorization, finished product nylon acid two is obtained by filtration（2- second
Base）Own ester.
Preferably, catalyst is tetramethoxy titanate ester, tetraethyl titanate, tetra-n-butyl titanate, tetraisopropyl titanate, metatitanic acid
One or more mixtures in four monooctyl esters, metatitanic acid tetraphenyl ester.
Preferably, water entrainer is 2-Ethylhexyl Alcohol, one or more mixtures in normal octane, dimethylbenzene.
Preferably, the lye that caustic scrubbing step uses is 2~3% sodium hydroxide solution of mass concentration, mass concentration 2~3%
Potassium hydroxide solution, 5~8% calcium hydroxide solution of mass concentration, 5~8% sodium carbonate liquor of mass concentration, mass concentration 5~
One or more mixed alkali liquors in 8% solution of potassium carbonate.
Preferably, decolorising agent can be one or more mixtures in atlapulgite, diatomite, activated carbon.
A kind of nylon acid two（2- ethyls）The preparation method of own ester, reaction principle are：
N=2~4 in formula, what is represented respectively is succinic acid, glutaric acid and adipic acid, i.e., mixed dibasic acid nylon acid is main
Ingredient.2-Ethylhexyl Alcohol is commonly called as industrial octanol, and maximum purposes is for manufacturing production plasticizer, such as phthalic acid
Dioctyl ester（DOP）, dioctyl terephthalate（DOTP）, trioctyl trimellitate (TOTM)（TOTM）, dioctyl adipate（DOA）, the last of the ten Heavenly stems
Adipate（DOS）.
The reaction mechanism is carried out in two steps, and under the conditions of titanate catalyst, the first step is by nylon acid and 2-Ethylhexyl Alcohol
Reaction generation nylon acid list（2- ethyls）Own ester, this step rapid reaction are completed.Second step be reaction rate-determining steps, nylon acid
It is single（2- ethyls）Own ester continuation is reacted with 2-Ethylhexyl Alcohol, generates nylon acid two（2- ethyls）Own ester.
Nylon acid is typical esterification with reacting for 2-Ethylhexyl Alcohol, belongs to reversible reaction, thus for make balance to
Complete direction movement is esterified, needs a kind of excessive reactant so that another reactant is converted into product to the greatest extent, carries
The conversion ratio of height reaction improves the conversion ratio of nylon acid using the method for excessive 2-Ethylhexyl Alcohol in of the invention.It is reacting simultaneously
It needs to remove the water generated in reaction process in time in the process, water entrainer can be added in, according to water entrainer with being produced in reaction process
Raw water forms azeotropic system, and water is removed system in time, makes esterification complete.
Advantageous effect of the present invention：
The present invention prepares a kind of novel environment friendly cold-resistant plasticizer, adds using the by-product nylon acid of industrial production adipic acid as raw material
It is added in plasticizer formula and uses, not only reduced the production cost of rubber and plastic enterprise, but also so that nylon acid is utilized well, together
When solve the problems, such as waste pollution environment, have very big economic benefit and social benefit.
Simple production process of the present invention, raw material is cheap and easy to get, and yield is high, does not need to special reaction, isolates and purifies equipment,
Industrialized production is very suitable for, for the enterprise of general production plasticizer, existing workshop and equipment can be used straight
Tap into capable production.
Nylon acid two produced by the invention（2- ethyls）Own ester has the advantages that and PVC compatibilities are good, cold resistance is excellent, full
The application requirement of sufficient plastic processing product.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Fig. 2 is gas phase analysis chromatogram.
Fig. 3 is gas phase analysis chromatography result table.
Specific embodiment
In order to preferably implement the present invention, spy gives an actual example explanation, but is not limitation of the present invention.
Embodiment 1：
2.5kg solid nylons acid is added in the reaction kettle of 10L（Henan table mountain Shen Ma groups provide）With 6.5kg industry octanols
（2-Ethylhexyl Alcohol）, stirring is started, is warming up to 80 DEG C, is filtered after material is completely dissolved through filter, by product pump to esterifying kettle,
0.9kg octanols are added as water entrainer, start agitating and heating heating, after starting reflux in water knockout drum and taking the water in system out of,
3g tetra-n-butyl titanates are added in, start esterification.The esterification water generated in reaction process is evaporated with 2-Ethylhexyl Alcohol, through cold
It is constantly separated in water knockout drum lower part after solidifying, the 2-Ethylhexyl Alcohol on upper strata is back to esterifying kettle.Treat that reaction to the 6th hour, is added
1.5g tetra-n-butyl titanates continue to be esterified.Esterification carries out 8 hours, sampling detecting acid number, during acid value≤1mgKOH/g, esterification
Reach terminal, stop reaction.
Material is transferred to dealcoholysis kettle, opens vacuum pump, deviates from excessive 2-Ethylhexyl Alcohol, and the 2-Ethylhexyl Alcohol of abjection can be
It is reused in above-mentioned esterification.Dealcoholysis process carries out under 0.094~0.096MPa of vacuum degree, when dealcoholysis temperature rises to
At 210 DEG C, stop heating, dealcoholysis terminates.The ester liquid that dealcoholysis terminates is entered into rectifying still, condition of high vacuum degree 0.096~
200~240 DEG C of fractions are collected under 0.098MPa, obtain thick ester sample.
Thick ester sample enters alkali cleaning kettle, adds in the sodium carbonate liquor of 1000g mass fractions 8%, stirring is started, in temperature 60
Alkali cleaning 20min at DEG C, then stratification, the ester liquid on upper strata enter washing kettle.1600g softened waters are added in, stirring are started, in temperature
20min is washed at 90 DEG C of degree, then stratification.
The ester liquid on the upper strata of stratification after washing is entered into air lift kettle, opens vacuum pump, condition of high vacuum degree 0.096~
Under the conditions of 0.098MPa, 1000g vapor, 140 DEG C of steam temperature are slowly introducing, air lift operation temperature is 155 DEG C.Air lift knot
Shu Hou adds in 2.5g atlapulgites, opens vacuum pump, under 0.094~0.096MPa of vacuum degree, heating dehydration, when temperature liter
During to 135 DEG C, stop heating, dehydration terminates, and finished product nylon acid two is obtained by filtration（2- ethyls）Own ester, weigh 6500g, and product is received
Rate 98%.
The nylon acid two of gained（2- ethyls）The index of correlation of own ester is as shown in the table：
| Serial number | Quality index | Unit | Detection method | Testing result |
| 1 | Appearance | Range estimation | Colourless transparent oil liquid | |
| 2 | Color and luster | Platinum cobalt colorimetric | GB/T 9282.1-2008 | 30 |
| 3 | Acid value | mgKOH/g | GB/T 6743-2008 | 0.088 |
| 4 | Moisture | % | GB/T 606-2003 | 0.039 |
| 5 | Content | % | GB/T 9722-2006 | 99 |
Embodiment 2：
2.5kg solid nylons acid is added in the reaction kettle of 10L（Henan table mountain Shen Ma groups provide）With 6.5kg industry octanols
（2-Ethylhexyl Alcohol）, stirring is started, is warming up to 80 DEG C, is filtered after material is completely dissolved through filter, by product pump to esterifying kettle,
Add 0.9kg normal octanes as water entrainer, start agitating and heating heating, after starting reflux in water knockout drum and taking the water in system out of,
3g tetra-n-butyl titanates are added in, start esterification.The esterification water generated in reaction process is condensed with the evaporation of water entrainer
It is constantly separated in water knockout drum lower part afterwards, the 2-Ethylhexyl Alcohol on upper strata is back to esterifying kettle.Treat that reaction to the 6th hour, adds 1.5g
Tetra-n-butyl titanate continues to be esterified.Esterification carries out 8 hours, sampling detecting acid number, and during acid value≤1mgKOH/g, esterification reaches
Terminal stops reaction.
Material is transferred to dealcoholysis kettle, opens vacuum pump, deviates from excessive 2-Ethylhexyl Alcohol and normal octane, the 2- ethyl hexyls of abjection
Alcohol and normal octane can recycle in above-mentioned esterification.Dealcoholysis process carries out under 0.094~0.096MPa of vacuum degree,
When dealcoholysis temperature rises to 210 DEG C, stop heating, dealcoholysis terminates.The ester liquid that dealcoholysis terminates is entered into rectifying still, in Gao Zhen
200~240 DEG C of fractions are collected under 0.096~0.098MPa of reciprocal of duty cycle, obtain thick ester sample.
Thick ester sample enters alkali cleaning kettle, adds in the sodium hydroxide solution of 1000g mass fractions 3%, stirring is started, in temperature
Alkali cleaning 20min at 60 DEG C, then stratification, the ester liquid on upper strata enter washing kettle.1600g softened waters are added in, start stirring,
20min is washed at 90 DEG C of temperature, then stratification.
The ester liquid on the upper strata of stratification after washing is entered into air lift kettle, opens vacuum pump, condition of high vacuum degree 0.096~
Under the conditions of 0.098MPa, 900g vapor, 140 DEG C of steam temperature are slowly introducing, air lift operation temperature is 155 DEG C.Air lift knot
Shu Hou adds in 2.5g activated carbons, opens vacuum pump, under 0.094~0.096MPa of vacuum degree, heating dehydration, when temperature rises to
At 135 DEG C, stop heating, dehydration terminates, and finished product nylon acid two is obtained by filtration（2- ethyls）Own ester, weigh 6500g, product yield
98%。
The nylon acid two of gained（2- ethyls）The index of correlation of own ester is as shown in the table：
| Serial number | Quality index | Unit | Detection method | Testing result |
| 1 | Appearance | Range estimation | Colourless transparent oil liquid | |
| 2 | Color and luster | Platinum cobalt colorimetric | GB/T 9282.1-2008 | 30 |
| 3 | Acid value | mgKOH/g | GB/T 6743-2008 | 0.074 |
| 4 | Moisture | % | GB/T 606-2003 | 0.030 |
| 5 | Content | % | GB/T 9722-2006 | 99 |
Claims (9)
1. a kind of nylon acid two（2- ethyls）The preparation method of own ester, it is characterised in that got a foothold with the by-product of industrial production adipic acid
It is raw material and 2-Ethylhexyl Alcohol to expect nylon acid（It is commonly called as industrial octanol）Esterification occurs, prepares high-quality nylon acid two（2- second
Base）Own ester.
2. a kind of nylon acid two according to claim 1（2- ethyls）The preparation method of own ester, it is characterised in that synthesis Buddhist nun
Imperial acid two（2- ethyls）The concrete operation step of own ester is as follows：
a）First nylon acid and 2-Ethylhexyl Alcohol are dissolved for 1: 2.1~1: 3.6 in dissolution kettle by the mass ratio that feeds intake, dissolving temperature
Degree control is filtered operation at 70~95 DEG C, by the material dissolved, removes the solid insoluble in nylon acid；
b）Material enters esterifying kettle, add in 0.1 ‰~1 ‰ catalyst of material gross mass, material gross mass 5~20%
Water entrainer, stirring heating start esterification, and at 170~240 DEG C, esterification time is controlled in 6~10 h for esterification temperature control,
Separate the water that esterification generates in reaction process from water knockout drum in time, until there is no water generation, while sampling analysis, survey esterification
Liquid acid value, until during acid value≤1mgKOH/g, esterification reaches terminal, you can stops reaction；
c）Material is transferred to dealcoholysis kettle, excessive 2-Ethylhexyl Alcohol is deviate under conditions of 0.094~0.096MPa of vacuum degree and with water
Agent, dealcoholysis temperature are 130~230 DEG C, and the 2-Ethylhexyl Alcohol and water entrainer of abjection return to esterifying kettle and reuse；
d）The ester liquid that dealcoholysis terminates enters rectifying still, and 200~240 DEG C are collected under 0.096~0.098MPa of condition of high vacuum degree
Fraction obtains thick ester sample；The front-end volatiles steamed before 200 DEG C, return in dissolution kettle and reuse；Distillation operation does not steam
Dry, distillation residual liquid is returned in dissolution kettle and is reused；
e）Thick ester sample enters alkali cleaning kettle, adds in lye, carries out alkali cleaning, and lye dosage is the thick ester production of 100~200kg lye/ton
Product, stratification, the ester liquid on upper strata enter washing kettle；Softened water is added in, the dosage of softened water is 200~300kg water/thick ester of ton
Product is washed, stratification, and the ester liquid on upper strata enters air lift kettle；The operation temperature of alkali cleaning and water-washing step is controlled 60
~90 DEG C；
f）Upper strata ester liquid pump after washing is entered into air lift kettle, high-temperature vapor is slowly introducing in air lift bottom portion, in condition of high vacuum degree
Under the conditions of slough a small amount of 2-Ethylhexyl Alcohol and low-boiling-point substance present in ester liquid；The 2-Ethylhexyl Alcohol taken out of during air lift returns to molten
It is reused in solution kettle；The steam temperature used is 140 DEG C, and the dosage of vapor is 100~150kg/ tons of thick esters, during air lift
Between for 2~3h, air lift operation temperature is 150~160 DEG C, and vacuum degree is 0.096~0.098MPa；
g）Ester liquid pump after air lift is entered into refining kettle, decolorising agent of the dosage for 0.2~0.6kg/ tons of products is added in, in vacuum degree
It is carried out under 0.094~0.096MPa, temperature is 120~140 DEG C, carries out dehydration and decolorization, finished product nylon acid two is obtained by filtration（2- second
Base）Own ester.
3. a kind of nylon acid two according to claim 2（2- ethyls）The preparation method of own ester, it is characterised in that catalyst
For in tetramethoxy titanate ester, tetraethyl titanate, tetra-n-butyl titanate, tetraisopropyl titanate, four monooctyl ester of metatitanic acid, metatitanic acid tetraphenyl ester
One or more mixtures.
4. a kind of nylon acid two according to claim 2（2- ethyls）The preparation method of own ester, it is characterised in that water entrainer
For one or more mixtures in 2-Ethylhexyl Alcohol, normal octane, dimethylbenzene.
5. a kind of nylon acid two according to claim 2（2- ethyls）The preparation method of own ester, it is characterised in that alkali cleaning walks
Suddenly the lye used is 2~3% sodium hydroxide solution of mass concentration, 2~3% potassium hydroxide solution of mass concentration, mass concentration 5
~8% calcium hydroxide solution, 5~8% sodium carbonate liquor of mass concentration, one kind in 5~8% solution of potassium carbonate of mass concentration or
A variety of mixed alkali liquors.
6. a kind of nylon acid two according to claim 2（2- ethyls）The preparation method of own ester, it is characterised in that softened water
Dosage is the thick ester product of 250kg water/ton.
7. a kind of nylon acid two according to claim 2（2- ethyls）The preparation method of own ester, it is characterised in that alkali cleaning
Temperature is 60~70 DEG C.
8. a kind of nylon acid two according to claim 2（2- ethyls）The preparation method of own ester, it is characterised in that washing
Temperature is 80~90 DEG C.
9. a kind of nylon acid two according to claim 2（2- ethyls）The preparation method of own ester, it is characterised in that for taking off
Toner can be one or more mixtures in atlapulgite, diatomite, activated carbon.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040246A (en) * | 2019-11-14 | 2020-04-21 | 东莞市世泰贸易有限公司 | Improved preparation method of dioctyl adipate |
| 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 |
| CN115872865A (en) * | 2022-12-12 | 2023-03-31 | 新疆天利高新石化股份有限公司 | Preparation method of dibasic acid ester |
| CN117486716A (en) * | 2023-12-28 | 2024-02-02 | 天津渤化澳佳永利化工有限责任公司 | DOA production method |
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| CN111040246A (en) * | 2019-11-14 | 2020-04-21 | 东莞市世泰贸易有限公司 | Improved preparation method of dioctyl adipate |
| 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 |
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