CN112062674A - Trioctyl trimellitate and preparation method thereof - Google Patents
Trioctyl trimellitate and preparation method thereof Download PDFInfo
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- CN112062674A CN112062674A CN201910500294.7A CN201910500294A CN112062674A CN 112062674 A CN112062674 A CN 112062674A CN 201910500294 A CN201910500294 A CN 201910500294A CN 112062674 A CN112062674 A CN 112062674A
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- trioctyl trimellitate
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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
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Trioctyl trimellitate comprises the following raw materials in parts by weight: 50-60 parts of trimellitic anhydride, 117-125 parts of isooctyl alcohol, 0.08-0.15 part of zinc-tin solid acid, 0.2-1.5 parts of tetrabutyl titanate composite catalyst, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of alumina. The invention has the advantages of high product yield, small catalyst consumption, short reaction time, simple process, small environmental pollution and the like.
Description
Technical Field
The invention belongs to the technical field related to plasticizer production, and particularly relates to trioctyl trimellitate and a preparation method thereof.
Background
Trioctyl trimellitate (TOTM) plasticizer is a heat-resistant and durable main plasticizer, has the advantages of polyester plasticizer and monomer plasticizer, and has the plasticizing efficiency and the processing performance similar to those of phthalate plasticizer; the compatibility, plasticizing performance and low-temperature performance of the polyester plasticizer are better than those of the polyester plasticizer; the electrical properties are excellent, but the oil resistance is slightly poor; the method is mainly used for producing 105-DEG C heat-resistant wire and cable materials and other products requiring heat resistance and durability, such as plates, sheets, gaskets and the like, and is suitable for various plastics, such as polyvinyl chloride, vinyl chloride copolymer, cellulose nitrate, ethyl cellulose butyrate, polymethyl methacrylate and the like. Can be used for heat-resistant and durable products such as heat-resistant electric wire and cable materials, plates, sheet gaskets and the like.
The second major use of trioctyl trimellitate is as a replacement for polychlorinated biphenyls (toxic materials) as power capacitor impregnation solutions. As the wire and cable industry in China is in orbit with international standards, the temperature resistance level of the cable in the telecommunication industry is improved to 105 ℃ according to the ISO standard, and the product has good insulating property, low volatility and small mobility, so that the product is widely applied to wires and cables, automobile interior decorative materials, temperature-resistant wire coatings, high-performance polyester, copper wire waterproof coatings for motors and environment-friendly high-level plastic products, the application requirement is increased day by day, and the market potential is very great. Production and consumption of trioctyl trimellitate are rapidly increased abroad, and the trioctyl trimellitate belongs to one of varieties with the fastest increase range in European and American plasticizer products.
Only a small amount of trioctyl trimellitate is put into production in China, and the quality and the yield of the product can not meet the requirements of downstream processing industry by the conventional solvent method and the sulfation process.
Disclosure of Invention
The invention aims to provide trioctyl trimellitate and a preparation method thereof aiming at the defects of the prior art.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: trioctyl trimellitate comprises the following raw materials in parts by weight: 50-60 parts of trimellitic anhydride, 117-125 parts of isooctyl alcohol, 0.08-0.15 part of zinc-tin solid acid, 0.2-1.5 parts of tetrabutyl titanate composite catalyst, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of alumina.
A process for preparing trioctyl trimellitate according to claim 1, comprising the steps of: (1) adding 50-60 parts of trimellitic anhydride and 117-125 parts of isooctanol into a reaction kettle, and adding 0.2-1.5 parts of tetrabutyl titanate composite catalyst and 0.08-0.15 part of zinc-tin solid acid into the reaction kettle when the temperature in the reaction kettle rises to 142-153 ℃;
(2) when the temperature in the reaction kettle rises to 199-204 ℃, continuously adding 0.4-1.2 parts of tetrabutyl titanate composite catalyst and 0.1-0.13 parts of zinc-tin solid acid into the reaction kettle;
(3) after the temperature in the reaction kettle is kept at 199-204 ℃ for 40-55 min, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of aluminum oxide are added into the reaction kettle;
(4) after the reaction is finished, pumping to negative pressure of-10 to-15 KPa for dealcoholization for 40-55 min;
(5) adding 15-23 parts of activated carbon and 15-23 parts of diatomite, stirring for 65-85 min, and decoloring and filter-pressing to obtain the product.
Further, in the steps (1) to (3), the stirring speed of stirring in the reaction kettle is controlled to be 390 to 730r/min, and the pressure in the kettle is controlled to be 113 to 126 KPa.
The invention has the beneficial effects that: the invention has the advantages of high product yield, small catalyst consumption, short reaction time, simple process, small environmental pollution and the like.
Detailed Description
Example 1: trioctyl trimellitate comprises the following raw materials in parts by weight: 50-60 parts of trimellitic anhydride, 117-125 parts of isooctyl alcohol, 0.08-0.15 part of zinc-tin solid acid, 0.2-1.5 parts of tetrabutyl titanate composite catalyst, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of alumina.
A process for preparing trioctyl trimellitate according to claim 1, comprising the steps of: (1) adding 50-60 parts of trimellitic anhydride and 117-125 parts of isooctanol into a reaction kettle, and adding 0.2-1.5 parts of tetrabutyl titanate composite catalyst and 0.08-0.15 part of zinc-tin solid acid into the reaction kettle when the temperature in the reaction kettle rises to 142-153 ℃;
(2) when the temperature in the reaction kettle rises to 199-204 ℃, continuously adding 0.4-1.2 parts of tetrabutyl titanate composite catalyst and 0.1-0.13 parts of zinc-tin solid acid into the reaction kettle;
(3) after the temperature in the reaction kettle is kept at 199-204 ℃ for 40-55 min, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of aluminum oxide are added into the reaction kettle;
(4) after the reaction is finished, pumping to negative pressure of-10 to-15 KPa for dealcoholization for 40-55 min;
(5) adding 15-23 parts of activated carbon and 15-23 parts of diatomite, stirring for 65-85 min, and decoloring and filter-pressing to obtain the product.
In the steps (1) - (3), the stirring speed of stirring in the reaction kettle is controlled to be 390-730 r/min, and the pressure in the kettle is 113-126 KPa.
Example 2: trioctyl trimellitate comprises the following raw materials in parts by weight: 50-60 parts of trimellitic anhydride, 117-125 parts of isooctyl alcohol, 0.08-0.15 part of zinc-tin solid acid, 0.2-1.5 parts of tetrabutyl titanate composite catalyst, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of alumina.
A process for preparing trioctyl trimellitate according to claim 1, comprising the steps of: (1) adding 50-60 parts of trimellitic anhydride and 117-125 parts of isooctanol into a reaction kettle, and adding 0.2-1.5 parts of tetrabutyl titanate composite catalyst and 0.08-0.15 part of zinc-tin solid acid into the reaction kettle when the temperature in the reaction kettle rises to 142-153 ℃;
(2) when the temperature in the reaction kettle rises to 199-204 ℃, continuously adding 0.4-1.2 parts of tetrabutyl titanate composite catalyst and 0.1-0.13 parts of zinc-tin solid acid into the reaction kettle;
(3) after the temperature in the reaction kettle is kept at 199-204 ℃ for 40-55 min, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of aluminum oxide are added into the reaction kettle;
(4) after the reaction is finished, pumping to negative pressure of-10 to-15 KPa for dealcoholization for 40-55 min;
(5) adding 15-23 parts of activated carbon and 15-23 parts of diatomite, stirring for 65-85 min, and decoloring and filter-pressing to obtain the product.
In the steps (1) - (3), the stirring speed of stirring in the reaction kettle is controlled to be 390-730 r/min, and the pressure in the kettle is 113-126 KPa.
Claims (3)
1. Trioctyl trimellitate is characterized by comprising the following raw materials in parts by weight: 50-60 parts of trimellitic anhydride, 117-125 parts of isooctyl alcohol, 0.08-0.15 part of zinc-tin solid acid, 0.2-1.5 parts of tetrabutyl titanate composite catalyst, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of alumina.
2. The method for preparing trioctyl trimellitate according to claim 1, comprising the steps of: (1) adding 50-60 parts of trimellitic anhydride and 117-125 parts of isooctanol into a reaction kettle, and adding 0.2-1.5 parts of tetrabutyl titanate composite catalyst and 0.08-0.15 part of zinc-tin solid acid into the reaction kettle when the temperature in the reaction kettle rises to 142-153 ℃;
(2) when the temperature in the reaction kettle rises to 199-204 ℃, continuously adding 0.4-1.2 parts of tetrabutyl titanate composite catalyst and 0.1-0.13 parts of zinc-tin solid acid into the reaction kettle;
(3) after the temperature in the reaction kettle is kept at 199-204 ℃ for 40-55 min, 1-3.5 parts of silicon dioxide and 0.6-1.4 parts of aluminum oxide are added into the reaction kettle;
(4) after the reaction is finished, pumping to negative pressure of-10 to-15 KPa for dealcoholization for 40-55 min;
(5) adding 15-23 parts of activated carbon and 15-23 parts of diatomite, stirring for 65-85 min, and decoloring and filter-pressing to obtain the product.
3. The method for preparing trioctyl trimellitate according to claim 2, wherein in the steps (1) to (3), the stirring speed of the stirring in the reaction kettle is controlled to be 390 to 730r/min, and the pressure in the kettle is controlled to be 113 to 126 KPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910500294.7A CN112062674A (en) | 2019-06-11 | 2019-06-11 | Trioctyl trimellitate and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910500294.7A CN112062674A (en) | 2019-06-11 | 2019-06-11 | Trioctyl trimellitate and preparation method thereof |
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| CN112062674A true CN112062674A (en) | 2020-12-11 |
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| CN201910500294.7A Pending CN112062674A (en) | 2019-06-11 | 2019-06-11 | Trioctyl trimellitate and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030652A (en) * | 2010-11-23 | 2011-04-27 | 无锡双象化学工业有限公司 | Industrialized production method for synthesizing trioctyl trimellitate through composite catalysis |
| CN108101783A (en) * | 2017-12-29 | 2018-06-01 | 珠海市高栏联合新材料有限公司 | A kind of preparation method of trioctyl trimellitate (TOTM) |
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- 2019-06-11 CN CN201910500294.7A patent/CN112062674A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102030652A (en) * | 2010-11-23 | 2011-04-27 | 无锡双象化学工业有限公司 | Industrialized production method for synthesizing trioctyl trimellitate through composite catalysis |
| CN108101783A (en) * | 2017-12-29 | 2018-06-01 | 珠海市高栏联合新材料有限公司 | A kind of preparation method of trioctyl trimellitate (TOTM) |
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Application publication date: 20201211 |