CN105541675A - Preparing method of dioctyl terephthalate - Google Patents
Preparing method of dioctyl terephthalate Download PDFInfo
- Publication number
- CN105541675A CN105541675A CN201510982982.3A CN201510982982A CN105541675A CN 105541675 A CN105541675 A CN 105541675A CN 201510982982 A CN201510982982 A CN 201510982982A CN 105541675 A CN105541675 A CN 105541675A
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- CN
- China
- Prior art keywords
- dioctyl terephthalate
- parts
- reactor
- sulphur trioxide
- hours
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/06—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with sulfuric acid or sulfur trioxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/42—Separation; Purification; Stabilisation; Use of additives
- C07C303/44—Separation; Purification
-
- 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
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
Abstract
The invention discloses a preparing method of dioctyl terephthalate, which is prepared by taking 90-100 parts by weight of dioctyl terephthalate, 15-20 parts by weight of sulfur trioxide and 0.2-0.3 part by weight of catalyst as raw materials to be subjected to sulfonation reaction, degassing, water washing, dehydrating and press filtering. The dioctyl terephthalate reacts after being subjected to the sulfonation reaction, thereby greatly improving the intermiscibility and thermal resistance of the dioctyl terephthalate and polyvinyl chloride.
Description
Technical field
The invention belongs to chemical field, be specifically related to a kind of dioctyl terephthalate and preparation method thereof.
Background technology
Polyvinyl chloride is the good general-purpose plastics of a kind of over-all properties, the polyvinyl chloride elastomerics of rubber like is obtained after particularly can adding a large amount of softening agent, over-all properties is better, but surface brightness is better, there is no elastomeric sub-light, be generally used for high DP PVC or partial cross-linked polyvinyl chloride resin at present, but effect not clearly.
Summary of the invention
Goal of the invention: the object of the invention is to for the deficiencies in the prior art, provides a kind of preparation method of dioctyl terephthalate.
Technical scheme: in order to reach foregoing invention object, the present invention has specifically come like this: a kind of preparation method of dioctyl terephthalate, is characterized in that, comprises the following steps:
(1) get the dioctyl terephthalate of parts by weight 90 ~ 100 parts, the catalyzer of the sulphur trioxide of 15 ~ 20 parts and 0.2 ~ 0.3 part imports reactor and carries out sulfonation reaction, and control temperature, at 80 ~ 120 DEG C, continues 3h;
(2) undertaken degassed by the dioctyl terephthalate processed through step (1), control pressure 4mPa, to reactor, the volume of sulphur trioxide is less than 1% stopping;
(3) step (2) gained intermediate is distilled, control pressure 2mPa, at 130 ~ 150 DEG C, continue 4 ~ 6 hours;
(4) washed by step (3) gained intermediate, the mass ratio adding the water yield and dioctyl terephthalate is 50 ~ 200:1;
(5) step (4) gained intermediate is dewatered, be less than 1% to intermediate aqueous amount, leave standstill 6 ~ 8 hours at normal temperatures and pressures, rear press filtration and get final product.
2, the preparation method of dioctyl terephthalate according to claim 1, is characterized in that, described catalyzer is dicumyl peroxide.
3, the preparation method of dioctyl terephthalate according to claim 2, is characterized in that, in described step (1), each composition weight number is the dioctyl terephthalate of 100 parts, the sulphur trioxide of 15 parts, the dicumyl peroxide of 0.2 part.
Beneficial effect: the present invention, compared with conventional art, reacts after dioctyl terephthalate sulfonation reaction, substantially increases intermiscibility and the thermotolerance of dioctyl terephthalate and polyvinyl chloride.
Embodiment
Embodiment 1:
Get the dioctyl terephthalate of parts by weight 90 parts, the dicumyl peroxide of the sulphur trioxide of 15 parts and 0.2 part imports reactor and carries out sulfonation reaction, and control temperature, at 80 ~ 120 DEG C, continues 3h; Import air in reactor, control pressure 4mPa, to reactor, the volume of sulphur trioxide is less than 1% stopping; Continue to distill gained intermediate, control pressure 2mPa, at 130 ~ 150 DEG C, continue 4 ~ 6 hours; Then wash gained intermediate, the mass ratio adding the water yield and dioctyl terephthalate is 50 ~ 200:1;
Finally intermediate is dewatered, be less than 1% to intermediate aqueous amount, leave standstill 6 ~ 8 hours at normal temperatures and pressures, rear press filtration and get final product.
Embodiment 2:
Get the dioctyl terephthalate of parts by weight 100 parts, the dicumyl peroxide of the sulphur trioxide of 20 parts and 0.3 part imports reactor and carries out sulfonation reaction, and control temperature, at 80 ~ 120 DEG C, continues 3h; Import air in reactor, control pressure 4mPa, to reactor, the volume of sulphur trioxide is less than 1% stopping; Continue to distill gained intermediate, control pressure 2mPa, at 130 ~ 150 DEG C, continue 4 ~ 6 hours; Then wash gained intermediate, the mass ratio adding the water yield and dioctyl terephthalate is 50 ~ 200:1;
Finally intermediate is dewatered, be less than 1% to intermediate aqueous amount, leave standstill 6 ~ 8 hours at normal temperatures and pressures, rear press filtration and get final product.
Embodiment 3:
Get the dioctyl terephthalate of parts by weight 95 parts, the dicumyl peroxide of the sulphur trioxide of 18 parts and 0.2 part imports reactor and carries out sulfonation reaction, and control temperature, at 80 ~ 120 DEG C, continues 3h; Import air in reactor, control pressure 4mPa, to reactor, the volume of sulphur trioxide is less than 1% stopping; Continue to distill gained intermediate, control pressure 2mPa, at 130 ~ 150 DEG C, continue 4 ~ 6 hours; Then wash gained intermediate, the mass ratio adding the water yield and dioctyl terephthalate is 50 ~ 200:1;
Finally intermediate is dewatered, be less than 1% to intermediate aqueous amount, leave standstill 6 ~ 8 hours at normal temperatures and pressures, rear press filtration and get final product.
Embodiment 4:
Get the dioctyl terephthalate of parts by weight 98 parts, the dicumyl peroxide of the sulphur trioxide of 16 parts and 0.3 part imports reactor and carries out sulfonation reaction, and control temperature, at 80 ~ 120 DEG C, continues 3h; Import air in reactor, control pressure 4mPa, to reactor, the volume of sulphur trioxide is less than 1% stopping; Continue to distill gained intermediate, control pressure 2mPa, at 130 ~ 150 DEG C, continue 4 ~ 6 hours; Then wash gained intermediate, the mass ratio adding the water yield and dioctyl terephthalate is 50 ~ 200:1;
Finally intermediate is dewatered, be less than 1% to intermediate aqueous amount, leave standstill 6 ~ 8 hours at normal temperatures and pressures, rear press filtration and get final product.
Embodiment 5:
Get the dioctyl terephthalate of parts by weight 96 parts, the dicumyl peroxide of the sulphur trioxide of 17 parts and 0.2 part imports reactor and carries out sulfonation reaction, and control temperature, at 80 ~ 120 DEG C, continues 3h; Import air in reactor, control pressure 4mPa, to reactor, the volume of sulphur trioxide is less than 1% stopping; Continue to distill gained intermediate, control pressure 2mPa, at 130 ~ 150 DEG C, continue 4 ~ 6 hours; Then wash gained intermediate, the mass ratio adding the water yield and dioctyl terephthalate is 50 ~ 200:1;
Finally intermediate is dewatered, be less than 1% to intermediate aqueous amount, leave standstill 6 ~ 8 hours at normal temperatures and pressures, rear press filtration and get final product.
Claims (3)
1. a preparation method for dioctyl terephthalate, is characterized in that, comprises the following steps:
(1) get the dioctyl terephthalate of parts by weight 90 ~ 100 parts, the catalyzer of the sulphur trioxide of 15 ~ 20 parts and 0.2 ~ 0.3 part imports reactor and carries out sulfonation reaction, and control temperature, at 80 ~ 120 DEG C, continues 3h;
(2) undertaken degassed by the dioctyl terephthalate processed through step (1), control pressure 4mPa, to reactor, the volume of sulphur trioxide is less than 1% stopping;
(3) step (2) gained intermediate is distilled, control pressure 2mPa, at 130 ~ 150 DEG C, continue 4 ~ 6 hours;
(4) washed by step (3) gained intermediate, the mass ratio adding the water yield and dioctyl terephthalate is 50 ~ 200:1;
(5) step (4) gained intermediate is dewatered, be less than 1% to intermediate aqueous amount, leave standstill 6 ~ 8 hours at normal temperatures and pressures, rear press filtration and get final product.
2. the preparation method of dioctyl terephthalate according to claim 1, is characterized in that, described catalyzer is dicumyl peroxide.
3. the preparation method of dioctyl terephthalate according to claim 2, is characterized in that, in described step (1), each composition weight number is the dioctyl terephthalate of 100 parts, the sulphur trioxide of 15 parts, the dicumyl peroxide of 0.2 part.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510982982.3A CN105541675A (en) | 2015-12-24 | 2015-12-24 | Preparing method of dioctyl terephthalate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510982982.3A CN105541675A (en) | 2015-12-24 | 2015-12-24 | Preparing method of dioctyl terephthalate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105541675A true CN105541675A (en) | 2016-05-04 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510982982.3A Pending CN105541675A (en) | 2015-12-24 | 2015-12-24 | Preparing method of dioctyl terephthalate |
Country Status (1)
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| CN (1) | CN105541675A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005145836A (en) * | 2003-11-12 | 2005-06-09 | Konishi Kagaku Ind Co Ltd | Method for producing alkali salt of alkyl sulfo-substituted aromatic carboxylate |
| CN101279940A (en) * | 2008-05-20 | 2008-10-08 | 北京金方博源科技发展有限公司 | Preparation of isophthalic acid-5-sulfonic acid, ester, salt and ester salt thereof |
| JP2012087111A (en) * | 2010-10-18 | 2012-05-10 | Monda Shashingata Seisakusho:Kk | Synthesis of dimethyl 2-sulfoterephthalate sodium, and addition to polycondensation system of dimethyl terephthalate and ethylene glycol |
| CN102633693A (en) * | 2012-03-22 | 2012-08-15 | 潍坊沃尔特化学有限公司 | Method for synthesizing dimethyl isophthalate-5-sodium sulfonate |
| CN102911389A (en) * | 2012-11-01 | 2013-02-06 | 喻小琦 | Polythiophene composite material and preparation method thereof |
| 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 |
-
2015
- 2015-12-24 CN CN201510982982.3A patent/CN105541675A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005145836A (en) * | 2003-11-12 | 2005-06-09 | Konishi Kagaku Ind Co Ltd | Method for producing alkali salt of alkyl sulfo-substituted aromatic carboxylate |
| CN101279940A (en) * | 2008-05-20 | 2008-10-08 | 北京金方博源科技发展有限公司 | Preparation of isophthalic acid-5-sulfonic acid, ester, salt and ester salt thereof |
| JP2012087111A (en) * | 2010-10-18 | 2012-05-10 | Monda Shashingata Seisakusho:Kk | Synthesis of dimethyl 2-sulfoterephthalate sodium, and addition to polycondensation system of dimethyl terephthalate and ethylene glycol |
| CN102633693A (en) * | 2012-03-22 | 2012-08-15 | 潍坊沃尔特化学有限公司 | Method for synthesizing dimethyl isophthalate-5-sodium sulfonate |
| CN102911389A (en) * | 2012-11-01 | 2013-02-06 | 喻小琦 | Polythiophene composite material and preparation method thereof |
| 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 (1)
| Title |
|---|
| 孙永泰: ""对苯二甲酸二辛酯的合成工艺及应用"", 《聚酯工业》 * |
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Application publication date: 20160504 |
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