CN103664618A - Novel synthesis process of octyl 2-propylheptyl phthalate - Google Patents

Novel synthesis process of octyl 2-propylheptyl phthalate Download PDF

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Publication number
CN103664618A
CN103664618A CN201310612400.3A CN201310612400A CN103664618A CN 103664618 A CN103664618 A CN 103664618A CN 201310612400 A CN201310612400 A CN 201310612400A CN 103664618 A CN103664618 A CN 103664618A
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China
Prior art keywords
reaction
phthalate
alcohol
phthalic acid
octanol
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Pending
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CN201310612400.3A
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Chinese (zh)
Inventor
张桂琴
刘雪强
周旭楚
姚文超
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ZHEJIANG HAILIYE TECHNOLOGY Co Ltd
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ZHEJIANG HAILIYE TECHNOLOGY Co Ltd
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Priority to CN201310612400.3A priority Critical patent/CN103664618A/en
Publication of CN103664618A publication Critical patent/CN103664618A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation 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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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

The invention discloses a novel synthesis process of octyl 2-propylheptyl phthalate. The process comprises steps as follows: (1), raw materials are taken in a molar ratio of phthalate to alcohol of 1: (2.5-2.7), a catalyst, namely, titanium, is taken according to the amount accounting for 0.3%-0.35% of the total mass of phthalate and alcohol, and alcohol is a mixture of heptanol and octanol in a molar ratio of 1:1; (2), all phthalate, all heptanol and 50% of the catalyst are put into a reaction kettle, nitrogen is fed into the reaction kettle, and the reaction kettle is heated to the temperature of 200-220 DEG C for reaction; (3), all octanol and the residual catalyst are put into the reaction kettle, the reaction continues, and a crude product is obtained until a complete reaction is finished; and (4) after the crude product is washed with water and dealcoholized, activated carbon is used for decoloration, and a finished product is obtained after impurities are filtered. According to the process, nitrogen is used for protection, the condition that an esterification reaction is oxidized at the high temperature is prevented, the chroma grade of octyl 2-propylheptyl phthalate synthetized with the process is better, and the product quality is more stable.

Description

The new synthesis process of the pungent fat of a kind of phthalic acid (2-propyl group heptan)
Technical field
The present invention relates to organic chemical synthesis field, more specifically the synthesis technique of the pungent fat of a kind of plasticizer phthalic acid (2-propyl group heptan).
Background technology:
The pungent fat of phthalic acid (2-propyl group heptan) is the industrial softening agent of master that a kind of electrical property is good, plasticizing efficiency is high.It has good winter hardiness, thermotolerance and resistance to extractable, is applicable to polyvinyl chloride (PVC) RESINS industrial processes, is particularly useful for heat-resisting cable material as required the application of the aspects such as the high CABLE MATERIALS insulating, transparent plastics particle, lamp box film.The pungent fat of phthalic acid (2-propyl group heptan) combines DOP and the advantage of DPHP in application, is the comprehensive primary plasticizer of a kind of performance.
The synthetic esterification that belongs to of the pungent fat of phthalic acid (2-propyl group heptan), the temperature of reaction of esterification is very high, easily causes oxidizing reaction, thereby affects quality and the colourity of product, and production cost is improved.
Summary of the invention:
For above-mentioned deficiency, the object of the present invention is to provide a kind of new synthesis process of the not oxidizable and pungent fat of the good phthalic acid of product colourity (2-propyl group heptan).
The present invention is achieved by the following technical solutions.
A new synthesis process for the pungent fat of phthalic acid (2-propyl group heptan), its processing step is:
(1) by phthalic acid: alcohol mol ratio is that 1:2.5-2.7 gets raw material, gets catalyst Ti isopropyl propionate by the 0.3%-0.35% of the total mass of phthalic acid and alcohol; Described alcohol is the mixture of enanthol and octanol, and enanthol: the mol ratio of octanol is 1:1;
(2) catalyzer of whole phthalic acids and enanthol and 50% is fed in reactor, in reactor, passes into nitrogen, be warming up to 200-220 ℃ of reaction;
(3) catalyzer of whole octanols and remaining 50% is fed in reactor and continues reaction, obtain crude product to complete reaction;
(3) crude product after having reacted is washed, after dealcoholysis, then is added 1% gac of reaction system total mass to decolour, and obtains the pungent fat of finished product phthalic acid (2-propyl group heptan) after impurity screening.
Beneficial effect: adopted nitrogen protection in this technique, prevented that esterification is at high temperature oxidized, better by the pungent fat colourity grade of the synthetic phthalic acid of this technique (2-propyl group heptan), quality product is more stable.
Embodiment:
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1:
Get 1640 kilograms of phthalic acids, 1508 kilograms of enanthol, 1690 kilograms of octanols, 14.6 kilograms of isopropyl titanates are standby; First the catalyst Ti isopropyl propionate of whole phthalic acids and enanthol and 7.3 kilograms is fed in reactor, in reactor, pass into nitrogen protection, material in reactor is warming up to 200-210 ℃, react after 2 hours, the octanol of 1690 kilograms and remaining isopropyl titanate are joined to continuation reaction in reactor until reaction finishes; Crude product is neutralized after washing, dealcoholysis, add the thick gac of 48.6 kilograms to decolour, after refiltering, obtain the pungent fat of finished product phthalic acid (2-propyl group heptan).

Claims (1)

1. a new synthesis process for the pungent fat of phthalic acid (2-propyl group heptan), is characterized in that: processing step is
(1) by phthalic acid: alcohol mol ratio is that 1:2.5-2.7 gets raw material, gets catalyst Ti isopropyl propionate by the 0.3%-0.35% of the total mass of phthalic acid and alcohol; Described alcohol is the mixture of enanthol and octanol, and enanthol: the mol ratio of octanol is 1:1;
(2) catalyzer of whole phthalic acids and enanthol and 50% is fed in reactor, in reactor, passes into nitrogen, be warming up to 200-220 ℃ of reaction;
(3) catalyzer of whole octanols and remaining 50% is fed in reactor and continues reaction, obtain crude product to complete reaction;
(3) crude product after having reacted is washed, after dealcoholysis, then is added 1% gac of reaction system total mass to decolour, and obtains the pungent fat of finished product phthalic acid (2-propyl group heptan) after impurity screening.
CN201310612400.3A 2013-11-28 2013-11-28 Novel synthesis process of octyl 2-propylheptyl phthalate Pending CN103664618A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310612400.3A CN103664618A (en) 2013-11-28 2013-11-28 Novel synthesis process of octyl 2-propylheptyl phthalate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310612400.3A CN103664618A (en) 2013-11-28 2013-11-28 Novel synthesis process of octyl 2-propylheptyl phthalate

Publications (1)

Publication Number Publication Date
CN103664618A true CN103664618A (en) 2014-03-26

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310612400.3A Pending CN103664618A (en) 2013-11-28 2013-11-28 Novel synthesis process of octyl 2-propylheptyl phthalate

Country Status (1)

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CN (1) CN103664618A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105111076A (en) * 2015-08-31 2015-12-02 山东蓝帆化工有限公司 Preparation method and application of dipropylheptyl sebacate
CN105330543A (en) * 2015-10-19 2016-02-17 中国石油化工股份有限公司 Refining processing method of polyol esters
CN113292425A (en) * 2021-06-17 2021-08-24 浙江皇星化工股份有限公司 Production method of bis (2-propyl) heptyl terephthalate

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105111076A (en) * 2015-08-31 2015-12-02 山东蓝帆化工有限公司 Preparation method and application of dipropylheptyl sebacate
CN105330543A (en) * 2015-10-19 2016-02-17 中国石油化工股份有限公司 Refining processing method of polyol esters
CN113292425A (en) * 2021-06-17 2021-08-24 浙江皇星化工股份有限公司 Production method of bis (2-propyl) heptyl terephthalate

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Addressee: Yang Jian

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Application publication date: 20140326