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Method for synthesizing fluorochloro succinic acid

A technology of fluorochlorosuccinic acid and fluorochlorocyclobutene, which is applied in chemical instruments and methods, oxidative preparation of carboxylic acids, organic chemistry, etc., can solve problems such as long routes, low reaction yields, and expensive raw materials, and achieve Simple product separation and purification, safe synthesis process and high product yield

Inactive Publication Date: 2018-02-23
CIVIL AVIATION UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw materials of this method are expensive, the reaction steps are long, and the reaction yield is low
[0004] As can be seen from the above, when preparing fluorochlorosuccinic acid, there are long routes, harsh conditions, and the disadvantages that raw materials are not easy to prepare, etc., which limit the industrialized production of fluorochlorosuccinic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Preparation of ring fluorination catalyst: adopt co-precipitation method, the steps are as follows, CrCl 3 , Cu(NO 3 ) 2 , Zn(NO 3 ) 2 The solution is mixed into a mixed solution at a molar ratio of 85:10:5, then ammonia water accounting for 30% by weight of the mixed solution is added dropwise to the above mixed solution, the pH value of the mixed solution is adjusted to 9.0, and after 24 hours of precipitation aging, the precipitation filtering, washing with deionized water, drying, and pressing to obtain a Cr-Cu-Zn catalyst.

[0024] The drying process of Cr-Cu-Zn catalyst: 20ml Cr-Cu-Zn catalyst is loaded into the fixed-bed reactor, and then the fixed-bed reactor is heated with an open tube heating furnace. Under the protection of 50ml / min nitrogen, the Cr-Cu-Zn catalyst is first raised to a temperature of 400°C at a rate of 10°C / min and dried for 10 hours, and then the temperature is lowered to 200°C, thereby completing the Cr-Cu-Zn catalyst drying process...

Embodiment 2

[0029] (1) Preparation of ring fluorination catalyst: adopt co-precipitation method, the steps are as follows, CrCl 3 , Ni(NO 3 ) 3 , In(NO 3 ) 3 The solution is mixed into a mixed solution at a molar ratio of 85:10:5, then ammonia water accounting for 30% by weight of the mixed solution is added dropwise to the above mixed solution, the pH value of the mixed solution is adjusted to 9.0, and after 24 hours of precipitation aging, the precipitation filtering, washing with deionized water, drying, and pressing to obtain a Cr-Ni-In catalyst.

[0030] Drying process of Cr-Ni-In catalyst: 20ml Cr-Ni-In catalyst is loaded into the fixed bed reactor, then the fixed bed reactor is heated with an open tube heating furnace. Under the protection of 50m / minl nitrogen, the Cr-Ni-In catalyst is first raised to 400°C at a rate of 10°C / min and dried for 10 hours, and then the temperature is lowered to 200°C to complete the Cr-Ni-In catalyst drying process.

[0031] Activation process of...

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PUM

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Abstract

The invention relates to a method for synthesizing fluorochloro succinic acid, and belongs to the field of organic chemical synthesis. The method for synthesizing fluorochloro succinic acid is characterized in that hexachlorobutadiene (the molecular formula is as follow: CCl2 being equal to CCl-CCl being equal to CCl2) generates fluorochloro cyclobutene (the molecular formula is as follow: Cyclo-C2FxCly-CCl being equal to CCl-, wherein the sum of the x and y is 4) under the effect of cyclo-fluorinated catalysts; then, the fluorochloro succinic acid (the molecular formula is HOOC-C2FxCly-COOH)is generated under the effect of oxidizing agents. CCl2 is equal to CCl-CCl being equal to CCl2 arrow Cyclo-C2FxCly-CCl being equal to CCl- arrow HOOC-C2FxCly-COOH. The method has the advantages thatthe raw materials are cheap; the resources can be conveniently obtained; the product separation and purification are simple; the industrial production is easy; three industrial wastes (waste water, waste solid and waste water) are few.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, in particular to a method for synthesizing fluorochlorosuccinic acid. Background technique [0002] Fluorochlorosuccinic acid has high industrial value and is a widely used industrial raw material. Its downstream products can be used to produce pentaheterocyclic compound alkyd resins, pesticides and insecticides, etc. It also has high application value in the synthesis of fluorine fine chemicals. According to reports, fluorochlorosuccinic acid has been widely used in the synthesis of new corrosion-resistant materials such as resins. [0003] At present, there are few reports on the synthesis of fluorochlorosuccinic acid. A method for synthesizing tetrafluorosuccinic acid is reported in the patent (US2438485), which generates tetrafluorosuccinic acid by oxidizing hexafluorocyclobutene. The raw materials of this method are difficult to prepare, which limits industrial producti...

Claims

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Application Information

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IPC IPC(8): C07C51/16C07C55/32B01J23/86
CPCB01J23/866B01J23/868C07C17/00C07C17/35C07C51/16C07C23/06C07C55/32
Inventor 周晓猛周彪赵洪海张青松
Owner CIVIL AVIATION UNIV OF CHINA
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