CN108101784A - A kind of preparation method of dioctyl adipate - Google Patents
A kind of preparation method of dioctyl adipate Download PDFInfo
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- CN108101784A CN108101784A CN201711483389.XA CN201711483389A CN108101784A CN 108101784 A CN108101784 A CN 108101784A CN 201711483389 A CN201711483389 A CN 201711483389A CN 108101784 A CN108101784 A CN 108101784A
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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
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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
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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Abstract
The present invention proposes a kind of preparation method of dioctyl adipate, adds in adipic acid and raw alcohol in a kettle, and then as the rise of temperature, catalyst butyl titanate and raw alcohol are put into reaction kettle in batch by being segmented；It is eventually adding SiO2And Al2O3, vacuum dealcoholysis after reaction adds in Na after dealcoholysis2CO3, it is eventually adding activated carbon and filters acquisition product.Catalyst and raw alcohol are added in several times in the present invention, catalyst butyl titanate is unlikely to deteriorate, the amount added in every time is by being precisely controlled, well solved in the prior art because butyl titanate as catalyst meet water easily decomposition and esterification can generate water, the problem of causing to need to add multi-catalyst and caused deterioration in quality in production process and improve volume resistivity, in addition, this invention also solves catalyst amount in DOA production processes it is excessive caused by production cost it is excessively high the problem of.
Description
Technical field
The present invention relates to the preparation methods of plasticizer, particularly relate to a kind of preparation method of dioctyl adipate.
Background technology
Dioctyl adipate (DOA) is a kind of cold-resistant plasticizer, can improve the low-temperature pliability of polymer and resistance to punching
Hitting property, the plasticizer being widely used as in agricultural film, artificial leather, Frozen Food Packaging, synthetic rubber.
In existing dioctyl adipate preparation process, because the butyl titanate as catalyst is easily met water decomposition and is sent out
Raw esterification simultaneously generates water.In order to tackle this problem, solution is that the more butyl titanates of addition are anti-to supplement
The butyl titanate that should fall, but add excessive butyl titanate and can cause deterioration in quality, in addition, such treating method
Production cost can be increased.
The content of the invention
In view of this, it is an object of the invention to propose a kind of preparation method of dioctyl adipate, which prevent preparations
The generation of butyl titanate mutability Geological Problems in the process, solves in dioctyl adipate production process that catalyst amount is excessive to be made
The problem of declining into product quality, and saved cost.
In order to solve the above technical problems, the goal of the invention of the present invention is achieved using following technical scheme：
A kind of preparation method of dioctyl adipate, includes the following steps：
S1,1000kg adipic acids and the raw alcohol of 2000-3000kg are put into reaction kettle；
S2, when temperature in reaction kettle rises to 100~115 DEG C, continue to add the metatitanic acid four of 0.8-2.0kg into reaction kettle
Butyl ester and 1.8~3.0kg raw alcohols；
S3, when temperature in reaction kettle rises to 125~135 DEG C, continue to add 1.5~3.5kg metatitanic acids four into reaction kettle
Butyl ester, 0.5~1.5kg, tri- isooctyl acid tin and 3.0~5.0kg raw alcohols；
S4, when temperature in reaction kettle rises to 160~170 DEG C, continue to add 1.5~3.5kg metatitanic acids four into reaction kettle
Butyl ester and 2.0~2.5kg raw alcohols；
S5, when temperature in reaction kettle rises to and is warming up to 190 DEG C, continue to add 0.3~1.5kg SiO into reaction kettle2
With 0.2~0.5kg Al2O3；
S6, treat that being evacuated to 1~10KPa after reaction keeps 20~50min vacuum dealcoholysis；
2~4m is added in after S7, dealcoholysis3The Na of 0.5~1.5% concentration2CO3；
S8, divide water after standing 15~30min, be warming up to 110~120 DEG C and be evacuated to 1~10KPa dehydrations；
S9, addition 30~50kg activated carbons are heated to 100~115 DEG C of 20~40min of stirring, and press filtration obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
Preferably, step S4a is further included after the step S4, treats that temperature rises to 170~177 DEG C in reaction kettle
When, start to add 0.3~0.6m of raw alcohol by fractionating column distributor3/ h preserves 1.3~1.5h.
Preferably, in the step S1-S5, mixer quickly stirs in reaction kettle, mixing speed 300-600r/
Min, pressure is in 101~115KPa in kettle.
Preferably, the raw alcohol is by pretreatment, specific method：Raw alcohol is taken to be warming up to 60 by heat exchanger
~75 DEG C for use.
Preferably, stirring should have frequency converter to carry out reversion 15min when kettle temperature rises to 190 DEG C.
The present invention have the advantage that compared with prior art for：Catalyst and raw alcohol are added several times in the present invention
Enter, catalyst butyl titanate is unlikely to deteriorate, the amount that adds in every time by being precisely controlled, well solved in the prior art because
For butyl titanate meets that water easily decomposes as catalyst and esterification can generate water, cause to need addition excessive in production process
Catalyst and the problem of cause deterioration in quality, in addition, this invention also solves catalyst amount in DOA production processes is excessive
Caused by production cost it is excessively high the problem of.
Specific embodiment
For those skilled in the art is allowed to become apparent from getting information about the present invention, the present invention will be made below further
Explanation.
Embodiment 1
A kind of preparation method of dioctyl adipate, includes the following steps：
S1,1000kg adipic acids and the raw alcohol of 2000kg are put into reaction kettle；
S2, when temperature in reaction kettle rises to 100 DEG C, continue to add into reaction kettle 0.8kg butyl titanate and
1.8kg raw alcohol；
S3, when temperature in reaction kettle rises to 125 DEG C, continue to add 1.5kg butyl titanates, 0.5kg into reaction kettle
Three isooctyl acid tin and 3.0kg raw alcohols；
S4, when temperature in reaction kettle rises to 160 DEG C, continue to add 1.5kg butyl titanates and 2.0kg into reaction kettle
Raw alcohol；
S4a, when temperature in reaction kettle rises to 170 DEG C, start to add raw alcohol 0.3m by fractionating column distributor3/ h is preserved
1.3h；
S5, when temperature in reaction kettle rises to and is warming up to 190 DEG C, continue to add 0.3kg SiO into reaction kettle2With
0.2kg Al2O3；
S6, treat that being evacuated to 10KPa after reaction keeps 20min vacuum dealcoholysis；
2m is added in after S7, dealcoholysis3The Na of 0.5% concentration2CO3；
S8, divide water after standing 15min, be warming up to 110 DEG C and be evacuated to 10KPa dehydrations；
S9, addition 30kg activated carbons are heated to 100 DEG C of stirring 20min, and press filtration obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
In the step S1-S5, mixer quickly stirs in reaction kettle, mixing speed 300-600r/min, kettle internal pressure
By force in 101~115KPa.
By pre-processing, specific method is the raw alcohol：Raw alcohol is taken to be warming up to 60~75 DEG C for use by heat exchanger.
Stirring should have frequency converter to carry out reversion 15min when kettle temperature rises to 190 DEG C.
Embodiment 2
A kind of preparation method of dioctyl adipate, includes the following steps：
S1,1000kg adipic acids and the raw alcohol of 3000kg are put into reaction kettle；
S2, when temperature in reaction kettle rises to 115 DEG C, continue to add into reaction kettle 2.0kg butyl titanate and
3.0kg raw alcohol；
S3, when temperature in reaction kettle rises to 135 DEG C, continue to add 3.5kg butyl titanates, 1.5kg into reaction kettle
Three isooctyl acid tin and 5.0kg raw alcohols；
S4, when temperature in reaction kettle rises to 170 DEG C, continue to add 3.5kg butyl titanates and 2.5kg into reaction kettle
Raw alcohol；
S4a, when temperature in reaction kettle rises to 177 DEG C, start to add raw alcohol 0.6m by fractionating column distributor3/ h is preserved
1.5h；
S5, when temperature in reaction kettle rises to and is warming up to 190 DEG C, continue to add 1.5kg SiO into reaction kettle2With
0.5kg Al2O3；
S6, treat that being evacuated to 1KPa after reaction keeps 50min vacuum dealcoholysis；
4m is added in after S7, dealcoholysis3The Na of 1.5% concentration2CO3；
S8, divide water after standing 30min, be warming up to 120 DEG C and be evacuated to 1KPa dehydrations；
S9, addition 50kg activated carbons are heated to 115 DEG C of stirring 40min, and press filtration obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
In the step S1-S5, mixer quickly stirs in reaction kettle, mixing speed 300-600r/min, kettle internal pressure
By force in 101~115KPa.
By pre-processing, specific method is the raw alcohol：Raw alcohol is taken to be warming up to 60~75 DEG C for use by heat exchanger.
Stirring should have frequency converter to carry out reversion 15min when kettle temperature rises to 190 DEG C.
Embodiment 3
A kind of preparation method of dioctyl adipate, includes the following steps：
S1,1000kg adipic acids and the raw alcohol of 2500kg are put into reaction kettle；
S2, when temperature in reaction kettle rises to 110 DEG C, continue to add into reaction kettle 1.5kg butyl titanate and
2.2kg raw alcohol；
S3, when temperature in reaction kettle rises to 130 DEG C, continue to add 2.0kg butyl titanates, 1.0kg into reaction kettle
Three isooctyl acid tin and 4.0kg raw alcohols；
S4, when temperature in reaction kettle rises to 165 DEG C, continue to add 2.0kg butyl titanates and 2.2kg into reaction kettle
Raw alcohol；
S4a, when temperature in reaction kettle rises to 175 DEG C, start to add raw alcohol 0.5m by fractionating column distributor3/ h is preserved
1.4h；
S5, when temperature in reaction kettle rises to and is warming up to 190 DEG C, continue to add 1.0kg SiO into reaction kettle2With
0.3kg Al2O3；
S6, treat that being evacuated to 10KPa after reaction keeps 30min vacuum dealcoholysis；
3m is added in after S7, dealcoholysis3The Na of 1.0% concentration2CO3；
S8, divide water after standing 20min, be warming up to 115 DEG C and be evacuated to 10KPa dehydrations；
S9, addition 40kg activated carbons are heated to 110 DEG C of stirring 30min, and press filtration obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
In the step S1-S5, mixer quickly stirs in reaction kettle, mixing speed 300-600r/min, kettle internal pressure
By force in 101~115KPa.
By pre-processing, specific method is the raw alcohol：Raw alcohol is taken to be warming up to 60~75 DEG C for use by heat exchanger.
Stirring should have frequency converter to carry out reversion 15min when kettle temperature rises to 190 DEG C.
The above description is merely a specific embodiment, but protection scope of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can readily occur in change or replacement, should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (5)
1. a kind of preparation method of dioctyl adipate, which is characterized in that include the following steps：
S1,1000kg adipic acids and the raw alcohol of 2000-3000kg are put into reaction kettle；
S2, when temperature in reaction kettle rises to 100~115 DEG C, continue to add the butyl titanate of 0.8-2.0kg into reaction kettle
With 1.8~3.0kg raw alcohols；
S3, when temperature in reaction kettle rises to 125~135 DEG C, continue to add into reaction kettle 1.5~3.5kg butyl titanates,
0.5~1.5kg, tri- isooctyl acid tin and 3.0~5.0kg raw alcohols；
S4, when temperature in reaction kettle rises to 160~170 DEG C, continue to add 1.5~3.5kg butyl titanates into reaction kettle
With 2.0~2.5kg raw alcohols；
S5, when temperature in reaction kettle rises to and is warming up to 190 DEG C, continue to add 0.3~1.5kg SiO into reaction kettle2With 0.2
~0.5kg Al2O3；
S6, treat that being evacuated to 1~10KPa after reaction keeps 20~50min vacuum dealcoholysis；
2~4m is added in after S7, dealcoholysis3The Na of 0.5~1.5% concentration2CO3；
S8, divide water after standing 15~30min, be warming up to 110~120 DEG C and be evacuated to -0.090~-0.099MPa dehydrations；
S9, addition 30~50kg activated carbons are heated to 100~115 DEG C of 20~40min of stirring, and press filtration obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
2. the preparation method of dioctyl adipate according to claim 1, which is characterized in that also wrapped after the step S4
Include step S4a, when temperature in reaction kettle rises to 170~177 DEG C, start by fractionating column distributor add raw alcohol 0.3~
0.6m3/ h preserves 1.3~1.5h.
3. the preparation method of dioctyl adipate according to claim 1 or 2, which is characterized in that the step S1-S5
In, mixer quickly stirs in reaction kettle, mixing speed 300-600r/min, and pressure is in 101~115KPa in kettle.
4. the preparation method of dioctyl adipate according to claim 1, which is characterized in that the raw alcohol is by pre- place
Reason, specific method are：Raw alcohol is taken to be warming up to 60~75 DEG C for use by heat exchanger.
5. the preparation method of dioctyl adipate according to claim 1, which is characterized in that stirring should have frequency converter in kettle
Temperature carries out reversion 15min when rising to 190 DEG C.
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| CN201711483389.XA CN108101784A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of dioctyl adipate |
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| CN201711483389.XA CN108101784A (en) | 2017-12-29 | 2017-12-29 | A kind of preparation method of dioctyl adipate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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| CN101139293A (en) * | 2007-08-17 | 2008-03-12 | 郭立耀 | Method for producing dioctyl terephthalate |
| CN102701984A (en) * | 2012-05-25 | 2012-10-03 | 安徽香枫新材料有限公司 | Production method of dioctyl terephthalate |
| CN102924279A (en) * | 2012-10-16 | 2013-02-13 | 江苏正丹化学工业股份有限公司 | Catalytic synthesis method of tri-octyl tri-meta-benzoate |
| CN104610063A (en) * | 2015-01-08 | 2015-05-13 | 宜兴市阳洋塑料助剂有限公司 | Novel preparation method of dioctyl terephthalate |
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2017
- 2017-12-29 CN CN201711483389.XA patent/CN108101784A/en not_active Withdrawn
Patent Citations (4)
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|---|---|---|---|---|
| CN101139293A (en) * | 2007-08-17 | 2008-03-12 | 郭立耀 | Method for producing dioctyl terephthalate |
| CN102701984A (en) * | 2012-05-25 | 2012-10-03 | 安徽香枫新材料有限公司 | Production method of dioctyl terephthalate |
| CN102924279A (en) * | 2012-10-16 | 2013-02-13 | 江苏正丹化学工业股份有限公司 | Catalytic synthesis method of tri-octyl tri-meta-benzoate |
| CN104610063A (en) * | 2015-01-08 | 2015-05-13 | 宜兴市阳洋塑料助剂有限公司 | Novel preparation method of dioctyl terephthalate |
Non-Patent Citations (2)
| Title |
|---|
| 傅梅绮: "对苯二甲酸二辛酯生产技术及工艺改进", 《天津化工》 * |
| 薛维文，等: "对苯二甲酸二辛醋生产工艺述评", 《福建化工》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Application publication date: 20180601 |