CN108863782A - A kind of preparation method of three monooctyl ester of trimesic acid - Google Patents
A kind of preparation method of three monooctyl ester of trimesic acid Download PDFInfo
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- CN108863782A CN108863782A CN201810638312.3A CN201810638312A CN108863782A CN 108863782 A CN108863782 A CN 108863782A CN 201810638312 A CN201810638312 A CN 201810638312A CN 108863782 A CN108863782 A CN 108863782A
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- reaction kettle
- raw alcohol
- trimesic acid
- monooctyl ester
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention proposes the preparation methods of three monooctyl ester of trimesic acid, and trimesic acid and raw alcohol are added in a kettle, then as the raising of temperature, put into catalyst-butyl titanate and raw alcohol into reaction kettle in batch by being segmented；It is eventually adding SiO2And Al2O3, Na is added after dealcoholysis in vacuum dealcoholysis after reaction2CO3, it is eventually adding active carbon and filters acquisition product.Catalyst and raw alcohol are added several times in the present invention, catalyst butyl titanate is unlikely to deteriorate, the amount being added every time is by being precisely controlled, it has well solved in the prior art because butyl titanate easily decomposes and esterification can generate water as catalyst chance water, has caused to need the problem of adding multi-catalyst and causing deterioration in quality in production process.Three monooctyl ester of trimesic acid is obviously improved compared to three monooctyl ester volume resistivity of trimellitic acid and flash-point in the present invention, is a kind of good new plasticizer.
Description
Technical field
The present invention relates to the preparation methods of plasticizer, particularly relate to a kind of preparation method of three monooctyl ester of trimesic acid.
Background technique
Trioctyl trimellitate (TOTM) (TOTM) plasticizer is a kind of heat-resisting and permanent seal cooling primary plasticizer, has both polyester plasticizer
And the advantages of monomeric plasticizer, plasticizing efficiency and processing performance are close with phthalic ester plasticizer；Compatibility, soffening
Energy, cryogenic property are excellent compared with polyester plasticizer；Excellent electrical properties, but oil resistivity is slightly poor；It is resistance to mainly for the production of 105 degrees Celsius of grades
Hot wire cable material and other require heat-resisting and durability plate, sheet material, the products such as gasket, be suitable for polyvinyl chloride,
A variety of plastics such as vinyl chloride copolymer, nitrocellulose, ethyl butyric acid cellulose, polymethyl methacrylate.It can be used for heat-resisting
Heat-resisting and durability the product such as wire cable material, plate, sheet material gasket.And three monooctyl ester of trimesic acid dodges on its basis
Point is higher, and volume resistivity is also obviously improved.
Summary of the invention
In view of this, which prevent systems it is an object of the invention to propose a kind of preparation method of three monooctyl ester of trimesic acid
The generation of butyl titanate mutability Geological Problems, solves catalyst amount mistake in three monooctyl ester production process of trimesic acid during standby
The problem of causing product quality to decline greatly, and improve volume resistivity and saved cost.
In order to solve the above technical problems, goal of the invention of the invention is achieved using following technical scheme：
A kind of preparation method of three monooctyl ester of trimesic acid, includes the following steps：
S1,1000kg trimesic acid and 1800~2500kg raw alcohol are put into reaction kettle；
S2, when temperature in reaction kettle rises to 120~135 DEG C, continue to add 1.2~2.5kg metatitanic acid four into reaction kettle
Butyl ester, 0.2~1.0kg, tri- isooctyl acid tin and 2.0~3.5kg raw alcohol；
S3, when temperature in reaction kettle rises to 155~165 DEG C, continue to add 2.2~4.0kg metatitanic acid four into reaction kettle
Butyl ester, 0.5~1.5kg, tri- isooctyl acid tin and 2.5~3.5kg raw alcohol；
S4, when temperature in reaction kettle rises to 180~185 DEG C, continue to add 2.0~3.5kg metatitanic acid four into reaction kettle
Butyl ester and 2.5~4.5kg raw alcohol；
S5, when temperature in reaction kettle rises to and is warming up to 205 DEG C, continue to add into reaction kettle 205 DEG C be added 0.8~
2.5kgSiO2With 0.4~1.0kgAl2O3；
S6, the dealcoholysis of 20~50min vacuum is kept to be evacuated to 1~10KPa after reaction；
2~4m is added 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 dehydration；
S9, addition 30~50kg active carbon are heated to 100~115 DEG C of 20~40min of stirring, and filters pressing obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
Preferably, further include step S3a after the step S3, rise to 170~177 DEG C to temperature in reaction kettle
When, start to add 0.3~0.6m of raw alcohol by fractionating column distributor3/ h saves 1.3~1.5h.
Preferably, in the step S1-S5, blender is quickly stirred 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 stand-by.
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 is added every time by being precisely controlled, well solved in the prior art because
Water is met as catalyst for butyl titanate easily to decompose and esterification can generate water, causes to need to add in production process excessive
Catalyst and the problem of cause deterioration in quality, in addition, making this invention also solves catalyst amount in production process is excessive
At the excessively high problem of production cost and improve volume resistivity.
Specific embodiment
The present invention is got information about to allow those skilled in the art to be more clear, the present invention will be made below further
Explanation.
Embodiment 1
A kind of preparation method of three monooctyl ester of trimesic acid, includes the following steps：
S1,1000kg trimesic acid and 1800kg raw alcohol are put into reaction kettle；
S2, when temperature in reaction kettle rises to 120 DEG C, continue to add 1.2kg butyl titanate, 0.2kg into reaction kettle
Three isooctyl acid tin and 2.0kg raw alcohol；
S3, when temperature in reaction kettle rises to 155 DEG C, continue to add 2.2kg butyl titanate, 0.5kg into reaction kettle
Three isooctyl acid tin and 2.5kg raw alcohol；
S3a, when temperature in reaction kettle rises to 170 DEG C, start by fractionating column distributor to add raw alcohol 0.3m3/ h is saved
1.5h；
S4, when temperature in reaction kettle rises to 180 DEG C, continue to add 2.0kg butyl titanate and 2.5kg into reaction kettle
Raw alcohol；
S5, when temperature in reaction kettle rises to and is warming up to 205 DEG C, continue to add 205 DEG C of additions into reaction kettle
0.8kgSiO2And 0.4kgAl2O3；
S6, the dealcoholysis of 50min vacuum is kept to be evacuated to 10KPa after reaction；
2m is added after S7, dealcoholysis3The Na of 1.5% concentration2CO3；
S8, divide water after standing 30min, be warming up to 110 DEG C and be evacuated to 10KPa dehydration；
S9, addition 30kg active carbon are heated to 100 DEG C of stirring 20min, and filters pressing obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
In the step S1-S5, blender is quickly stirred 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 three monooctyl ester of trimesic acid, includes the following steps：
S1,1000kg trimesic acid and 2500kg raw alcohol are put into reaction kettle；
S2, when temperature in reaction kettle rises to 135 DEG C, continue to add 2.5kg butyl titanate, 1.0kg into reaction kettle
Three isooctyl acid tin and 3.5kg raw alcohol；
S3, when temperature in reaction kettle rises to 165 DEG C, continue to add 4.0kg butyl titanate, 1.5kg into reaction kettle
Three isooctyl acid tin and 3.5kg raw alcohol；
S3a, when temperature in reaction kettle rises to 177 DEG C, start by fractionating column distributor to add raw alcohol 0.6m3/ h is saved
1.3h；
S4, when temperature in reaction kettle rises to 185 DEG C, continue to add 3.5kg butyl titanate and 4.5kg into reaction kettle
Raw alcohol；
S5, when temperature in reaction kettle rises to and is warming up to 205 DEG C, continue to add 205 DEG C of additions into reaction kettle
2.5kgSiO2And 1.0kgAl2O3；
S6, the dealcoholysis of 20min vacuum is kept to be evacuated to 1KPa after reaction；
4m is added after S7, dealcoholysis3The Na of 0.5% concentration2CO3；
S8, divide water after standing 15min, be warming up to 120 DEG C and be evacuated to 1KPa dehydration；
S9, addition 50kg active carbon are heated to 115 DEG C of stirring 40min, and filters pressing obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
In the step S1-S5, blender is quickly stirred 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 three monooctyl ester of trimesic acid, includes the following steps：
S1,1000kg trimesic acid and 2100kg raw alcohol are put into reaction kettle；
S2, when temperature in reaction kettle rises to 130 DEG C, continue to add 2.0kg butyl titanate, 0.8kg into reaction kettle
Three isooctyl acid tin and 3.0kg raw alcohol；
S3, when temperature in reaction kettle rises to 160 DEG C, continue to add 3.0kg butyl titanate, 1.0kg into reaction kettle
Three isooctyl acid tin and 3.0kg raw alcohol；
S3a, when temperature in reaction kettle rises to 170~177 DEG C, start by fractionating column distributor add raw alcohol 0.3~
0.6m3/ h saves 1.3~1.5h；
S4, when temperature in reaction kettle rises to 182 DEG C, continue to add 3.0kg butyl titanate and 3.5kg into reaction kettle
Raw alcohol；
S5, when temperature in reaction kettle rises to and is warming up to 205 DEG C, continue to add 205 DEG C of additions into reaction kettle
1.5kgSiO2And 0.6kgAl2O3；
S6, the dealcoholysis of 30min vacuum is kept to be evacuated to 5KPa after reaction；
3m is added after S7, dealcoholysis3The Na of 1.0% concentration2CO3；
S8, divide water after standing 25min, be warming up to 115 DEG C and be evacuated to 5KPa dehydration；
S9, addition 40kg active carbon are heated to 110 DEG C of stirring 30min, and filters pressing obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
In the step S1-S5, blender is quickly stirred 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 scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and 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 three monooctyl ester of trimesic acid, which is characterized in that include the following steps：
S1,1000kg trimesic acid and 1800~2500kg raw alcohol are put into reaction kettle；
S2, when temperature in reaction kettle rises to 120~135 DEG C, continue to add into reaction kettle 1.2~2.5kg butyl titanate,
0.2~1.0kg, tri- isooctyl acid tin and 2.0~3.5kg raw alcohol；
S3, when temperature in reaction kettle rises to 155~165 DEG C, continue to add into reaction kettle 2.2~4.0kg butyl titanate,
0.5~1.5kg, tri- isooctyl acid tin and 2.5~3.5kg raw alcohol；
S4, when temperature in reaction kettle rises to 180~185 DEG C, continue to add 2.0~3.5kg butyl titanate into reaction kettle
With 2.5~4.5kg raw alcohol；
S5, when temperature in reaction kettle rises to and is warming up to 205 DEG C, continue to add 205 DEG C of 0.8~2.5kg of addition into reaction kettle
SiO2With 0.4~1.0kgAl2O3；
S6, the dealcoholysis of 20~50min vacuum is kept to be evacuated to 1~10KPa after reaction；
2~4m is added 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 dehydration；
S9, addition 30~50kg active carbon are heated to 100~115 DEG C of 20~40min of stirring, and filters pressing obtains product；
Raw alcohol in the step S1 is one or more of octanol, amylalcohol or nonyl alcohol.
2. the preparation method of three monooctyl ester of trimesic acid according to claim 1, which is characterized in that after the step S3 also
Including step S3a, when temperature in reaction kettle rises to 170~177 DEG C, start by fractionating column distributor add raw alcohol 0.3~
0.6m3/ h saves 1.3~1.5h.
3. the preparation method of three monooctyl ester of trimesic acid according to claim 1 or 2, which is characterized in that the step S1-S5
In, blender quickly stirs in reaction kettle, mixing speed 300-600r/min, and pressure is in 101~115KPa in kettle.
4. the preparation method of three monooctyl ester of trimesic acid according to claim 1, which is characterized in that the raw alcohol is by pre-
Processing, 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 three monooctyl ester of trimesic acid according to claim 1, which is characterized in that stirring should have frequency converter to exist
Kettle temperature carries out reversion 15min when rising to 190 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810638312.3A CN108863782A (en) | 2018-06-20 | 2018-06-20 | A kind of preparation method of three monooctyl ester of trimesic acid |
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| CN201810638312.3A CN108863782A (en) | 2018-06-20 | 2018-06-20 | A kind of preparation method of three monooctyl ester of trimesic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112958065A (en) * | 2021-03-17 | 2021-06-15 | 江苏正丹化学工业股份有限公司 | Composite catalyst for producing dioctyl terephthalate, preparation method and application thereof |
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| 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 |
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| CN101139293A (en) * | 2007-08-17 | 2008-03-12 | 郭立耀 | Method for producing dioctyl terephthalate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112958065A (en) * | 2021-03-17 | 2021-06-15 | 江苏正丹化学工业股份有限公司 | Composite catalyst for producing dioctyl terephthalate, preparation method and application thereof |
| CN112958065B (en) * | 2021-03-17 | 2023-02-24 | 江苏正丹化学工业股份有限公司 | Composite catalyst for producing dioctyl terephthalate, preparation method and application thereof |
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Application publication date: 20181123 |