CN111040246A - Improved preparation method of dioctyl adipate - Google Patents
Improved preparation method of dioctyl adipate Download PDFInfo
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- CN111040246A CN111040246A CN201911109992.0A CN201911109992A CN111040246A CN 111040246 A CN111040246 A CN 111040246A CN 201911109992 A CN201911109992 A CN 201911109992A CN 111040246 A CN111040246 A CN 111040246A
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- parts
- dioctyl adipate
- octanol
- reaction kettle
- catalyst
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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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- 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
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
Abstract
The invention relates to an improved preparation method of dioctyl adipate, which comprises the steps of taking 8-12 parts of adipic acid, 8-12 parts of terephthalic acid, 8-12 parts of trimellitic anhydride, 0.5-5.5 parts of catalyst and 64-76 parts of n-octanol, feeding the materials into a reaction kettle, filling nitrogen, heating by using heat conduction oil, adding a proper amount of tetraisopropyl titanate, heating to 180 ℃ and 210 ℃, esterifying for 15-20 hours under normal pressure, cooling by using a condenser, adding a proper amount of liquid alkali diluted by using water IV to one in the reaction kettle, vacuumizing, supplementing water and dealcoholizing for three hours, and pressurizing by using a filter circulating pump until diatomite and activated carbon are filtered and decolored to obtain a finished product. Through adopting the adipic acid that cold resistance is strong, n-octanol, trimellitic anhydride that the heat resistance is strong to take the good terephthalic acid of plastification effect as the base material and stable in structure after the reaction of reaction kettle high temperature, thereby plastification effect, cold-resistant effect, heat-resisting effect have obtained comparatively obvious promotion in PVC hard material, but wide application in plasticizer technical field.
Description
Technical Field
The invention relates to the technical field of plasticizers, in particular to a preparation method of improved dioctyl adipate.
Background
According to the prior art, PVC products are soft and hard, wherein the cold resistance of the products can only be improved by directly adding dioctyl adipate when the hard polyvinyl chloride material needs to be plasticized, the plasticizing effect is poor, the heat resistance is poor, and the ideal effect can be achieved by matching other plasticizers. However, the prior art does not have a material which can meet the requirements.
Therefore, a plasticizer having good plasticizing, cold-resistant and heat-resistant effects is yet to be studied.
Disclosure of Invention
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
an improved dioctyl adipate preparation method comprises the steps of feeding 8-12 parts of adipic acid, 8-12 parts of terephthalic acid, 8-12 parts of trimellitic anhydride and 64-76 parts of n-octanol into a reaction kettle, filling nitrogen, heating to 120 ℃ by using steam, heating to 180 ℃ by using heat conduction oil, adding a proper amount of tetraisopropyl titanate, heating to 180 ℃ and 210 ℃, esterifying for about 15-20 hours under normal pressure, closing the nitrogen, cooling by using a condenser, adding a proper amount of liquid alkali diluted by using water IV to one into the reaction kettle, vacuumizing, replenishing water and dealcoholizing for three hours, cooling to 110 by using a condenser, adding a proper amount of liquid alkali diluted by using water IV to one into the reaction kettle, neutralizing, dehydrating for one hour to obtain an improved dioctyl adipate crude product, and pressurizing by using a filter circulating pump until diatomite and activated carbon are filtered and decolored to obtain a finished product.
Further, the catalyst is tetraisopropyl titanate.
Further, the content of the catalyst is 0.5-5.5 parts.
Further, during specific preparation, 20 parts of adipic acid, 20 parts of terephthalic acid, 10 parts of trimellitic anhydride, 45 parts of n-octanol and 5 parts of a catalyst are selected as main materials.
Further, during specific preparation, 19 parts of adipic acid, 8 parts of terephthalic acid, 8 parts of trimellitic anhydride, 40 parts of n-octanol and 4.5 parts of a catalyst are selected as main materials.
Further, during specific preparation, 22 parts of adipic acid, 22 parts of terephthalic acid, 12 parts of trimellitic anhydride, 46 parts of n-octanol and 3 parts of a catalyst are selected as main materials.
After the components and the preparation method are adopted, the invention has the following advantages:
through adopting the adipic acid that cold resistance is strong, n-octanol, the trimellitic anhydride that the heat resistance is strong to take the good terephthalic acid of plastification effect as the base material through reation kettle high temperature reaction back stable in structure, thereby make plastification effect, cold-resistant effect, heat-resisting effect obtain comparatively obvious promotion in PVC hard material.
Detailed Description
The present invention is described in further detail below.
Example one
An improved dioctyl adipate preparation method comprises the steps of feeding 8 parts of adipic acid, 8 parts of terephthalic acid, 8 parts of trimellitic anhydride, 0.5 part of catalyst and 64 parts of n-octanol into a reaction kettle, filling nitrogen, raising the temperature to 120 ℃ by using steam, raising the temperature to 180 ℃ by using heat conduction oil, adding a proper amount of tetraisopropyl titanate, raising the temperature to 180 ℃, esterifying for 15 hours under normal pressure, closing the nitrogen, cooling by using a condenser, adding a proper amount of liquid caustic soda diluted by using water IV to one into the reaction kettle, vacuumizing, replenishing water and dealcoholizing for three hours, reducing the temperature to 110, adding a proper amount of liquid caustic diluted by using water IV to one into the reaction kettle, neutralizing, dehydrating for one hour to obtain an improved dioctyl adipate crude product, and pressurizing by using a filter circulating pump until diatomite and activated carbon are filtered and decolored to obtain a finished product.
Wherein the catalyst is tetraisopropyl titanate.
The specific operation is as follows: when a certain amount of octanol is put into the reaction kettle, a stirrer in the reaction kettle is opened, the octanol is stirred at a low speed, adipic acid is continuously put into the reaction kettle, and then terephthalic acid and trimellitic anhydride are delivered into the reaction kettle. The liquid alkali selected in the preparation process is sodium hydroxide solution. Because octanol is flammable, smoke and fire are avoided during the production process.
Then, after adding sodium hydroxide and diluting, starting to inject nitrogen into the reaction kettle, introducing steam into the reaction kettle to heat up, when the temperature rises to 120 ℃, heating by using heat conduction oil, and stopping heating when the temperature reaches 180 ℃.
Example two
An improved dioctyl adipate preparation method comprises the steps of feeding 12 parts of adipic acid, 12 parts of terephthalic acid, 12 parts of trimellitic anhydride, 5.5 parts of catalyst and 76 parts of n-octanol into a reaction kettle, filling nitrogen, raising the temperature to 120 ℃ by using steam, raising the temperature to 180 ℃ by using heat conduction oil, adding a proper amount of tetraisopropyl titanate, raising the temperature to 210 ℃, esterifying for 20 hours under normal pressure, closing the nitrogen, cooling by using a condenser, adding a proper amount of liquid caustic soda diluted by using water IV to one into the reaction kettle, vacuumizing, replenishing water and dealcoholizing for three hours, reducing the temperature to 110, adding a proper amount of liquid caustic diluted by using water IV to one into the reaction kettle, neutralizing, dehydrating for one hour to obtain an improved dioctyl adipate crude product, and pressurizing by using a filter circulating pump until diatomite and activated carbon are filtered and decolored to obtain a finished product.
EXAMPLE III
An improved dioctyl adipate preparation method comprises the steps of feeding 10 parts of adipic acid, 10 parts of terephthalic acid, 10 parts of trimellitic anhydride, 5 parts of catalyst and 70 parts of n-octanol into a reaction kettle, filling nitrogen, raising the temperature to 120 ℃ by using steam, raising the temperature to 180 ℃ by using heat conduction oil, adding an appropriate amount of tetraisopropyl titanate, raising the temperature to 200 ℃, esterifying for 18 hours under normal pressure, closing the nitrogen, cooling by using a condenser, adding an appropriate amount of liquid caustic soda diluted by using water IV to one into the reaction kettle, vacuumizing, replenishing water and dealcoholizing for three hours, reducing the temperature to 110, adding an appropriate amount of liquid caustic diluted by using water IV to one into the reaction kettle, neutralizing, dehydrating for one hour to obtain an improved dioctyl adipate crude product, and pressurizing by using a circulating pump until diatomite and activated carbon are filtered and decolored to obtain a finished product.
Claims (5)
1. An improved preparation method of dioctyl adipate is characterized in that, during specific preparation, feeding 8-12 parts of adipic acid, 8-12 parts of terephthalic acid, 8-12 parts of trimellitic anhydride, 0.5-5.5 parts of catalyst and 64-76 parts of n-octanol into a reaction kettle, introducing nitrogen, heating to 120 ℃ by using steam, heating to 180 ℃ by using heat transfer oil, adding a proper amount of tetraisopropyl titanate, heating to 210 ℃ by using 180 ℃, esterifying for 15-20 hours under normal pressure, closing the nitrogen, cooling by using a condenser, adding a proper amount of liquid caustic soda diluted by using water IV to one into the reaction kettle, vacuumizing, supplementing water and dealcoholizing for three hours, after the temperature is reduced to 110 ℃, adding a proper amount of aqueous alkali diluted by four times to one for neutralization, dehydrating for one hour to obtain an improved dioctyl adipate crude product, and pressurizing by using a filter circulating pump until diatomite and active carbon are filtered and decolored to obtain a finished product.
2. The improved dioctyl adipate as recited in claim 1, wherein said catalyst is tetraisopropyl titanate.
3. The improved preparation method of dioctyl adipate as claimed in claim 1, wherein the main materials selected in the concrete preparation process comprise 12 parts of adipic acid, 12 parts of terephthalic acid, 12 parts of trimellitic anhydride, 5.5 parts of catalyst and 76 parts of n-octanol.
4. The improved preparation method of dioctyl adipate as claimed in claim 1, wherein 8 parts of adipic acid, 8 parts of terephthalic acid, 8 parts of trimellitic anhydride, 0.5 part of catalyst and 64 parts of n-octanol are selected as main materials during specific preparation.
5. The improved preparation method of dioctyl adipate as claimed in claim 1, wherein during specific preparation, 10 parts of adipic acid, 10 parts of terephthalic acid, 10 parts of trimellitic anhydride, 5 parts of catalyst and 70 parts of n-octanol are selected as main materials.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911109992.0A CN111040246A (en) | 2019-11-14 | 2019-11-14 | Improved preparation method of dioctyl adipate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911109992.0A CN111040246A (en) | 2019-11-14 | 2019-11-14 | Improved preparation method of dioctyl adipate |
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| CN111040246A true CN111040246A (en) | 2020-04-21 |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1636962A (en) * | 2003-03-26 | 2005-07-13 | 蒋平平 | Production process of plasticizer with multiple variety and low consumption |
| CN101993548A (en) * | 2010-09-30 | 2011-03-30 | 浙江嘉澳环保科技股份有限公司 | Environment-friendly composite plasticizer and preparation method |
| EP2810932A1 (en) * | 2013-06-06 | 2014-12-10 | ExxonMobil Chemical Patents Inc. | Improvements in or relating to plasticiser esters |
| CN105504347A (en) * | 2015-12-11 | 2016-04-20 | 安徽律正科技信息服务有限公司 | Light-resistant, heat-resistant and anti-aging plasticizer for plastics |
| CN106795324A (en) * | 2014-10-09 | 2017-05-31 | 巴斯夫欧洲公司 | The plasticizer composition of cycloalkyl ester and terephthalate comprising saturated dicarboxylic acid |
| 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 |
-
2019
- 2019-11-14 CN CN201911109992.0A patent/CN111040246A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1636962A (en) * | 2003-03-26 | 2005-07-13 | 蒋平平 | Production process of plasticizer with multiple variety and low consumption |
| CN101993548A (en) * | 2010-09-30 | 2011-03-30 | 浙江嘉澳环保科技股份有限公司 | Environment-friendly composite plasticizer and preparation method |
| EP2810932A1 (en) * | 2013-06-06 | 2014-12-10 | ExxonMobil Chemical Patents Inc. | Improvements in or relating to plasticiser esters |
| CN106795324A (en) * | 2014-10-09 | 2017-05-31 | 巴斯夫欧洲公司 | The plasticizer composition of cycloalkyl ester and terephthalate comprising saturated dicarboxylic acid |
| CN105504347A (en) * | 2015-12-11 | 2016-04-20 | 安徽律正科技信息服务有限公司 | Light-resistant, heat-resistant and anti-aging plasticizer for plastics |
| 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 |
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