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Method for preparing environment-friendly plasticizer by recycling waste resources

An environmentally friendly plasticizer and waste resource technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of high purity requirements, low product quality, waste of effective resources, etc., and achieve good color and luster. , Small scale of equipment investment, the effect of solving waste

Active Publication Date: 2015-04-08
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Technical problem to be solved: the purpose of this invention is to provide a method of recycling waste resources to prepare environmentally friendly plasticizers, effectively solving the waste of effective resources in alkali reduction wastewater, and realizing the recycling of waste resources; Plasticizer production has technical defects such as high requirements on the purity of PTA raw materials and low product quality, alleviating the impact of the oil crisis on the environmental protection plasticizer industry

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0020] (1) PTA crude material recovery, the alkali reduction waste water (pH value is 14, PTA sodium concentration is 5000mg / L) is transferred in the acid analysis tank with stirring device, adds sulfuric acid and constantly stirs, continues to separate out PTA solid, Until the pH of the wastewater is 3-5. The mixed solution is subjected to plate-and-frame filtration, and the filter cake is recovered PTA crude material. After testing, the water content of the PTA crude material is 30 wt%, and the pH value is 4.

[0021] (2) The preparation of DOTP, the above-mentioned reclaimed PTA crude material and octanol are added in the esterification reactor with alcohol-water separation device, the mass ratio of PTA crude material and iso-octanol is 1:1.5, and mechanical stirring is started Heating and dehydration, when the reaction temperature reaches 180°C, add the catalyst tetrabutyl titanate to carry out the esterification reaction, the amount added is 0.5% of the total mass of the ...

Embodiment 2

[0024] (1) PTA crude material recovery, the alkali reduction wastewater (pH value is 14, PTA concentration is 2000mg / L) is transferred to the acid analysis tank with stirring device, sulfuric acid is added slowly and stirred continuously, and PTA solid is continuously precipitated , until the wastewater pH is 3-5. The mixed solution is subjected to plate and frame filtration, and the filter cake is recovered PTA crude material. The water content of the PTA crude material is 45 wt% and the pH value is 3 after testing.

[0025] (2) The preparation of DOTP, the above-mentioned reclaimed PTA crude material and octanol are added in the esterification reactor with alcohol-water separation device, the mass ratio of PTA crude material and isooctyl alcohol is 1:2.3, open mechanical stirring to carry out Heating and dehydration, when the reaction temperature reaches 180°C, add the catalyst tetrabutyl titanate to carry out the esterification reaction, the amount added is 0.3% of the tota...

Embodiment 3

[0028] (1) PTA coarse material recovery, the alkali reduction wastewater (pH value is 14, PTA concentration is 1300mg / L) is transferred to the acid analysis tank with stirring device, sulfuric acid is added slowly and stirred continuously, and PTA solid is continuously precipitated , until the wastewater pH is 3-5. The mixed solution is filtered with a plate and frame, and the filter cake is recovered PTA crude material. The water content of the PTA crude material is 52wt% and the pH value is 1 after testing.

[0029](2) The preparation of DOTP, the above-mentioned reclaimed PTA crude material and octanol are added in the esterification reactor with alcohol-water separation device, the mass ratio of PTA crude material and iso-octanol is 1:1.4, open mechanical stirring to carry out Heating and dehydration, when the reaction temperature reaches 180°C, add the catalyst tetrabutyl titanate to carry out the esterification reaction, the amount added is 0.7% of the total mass of the ...

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Abstract

The invention relates to a method for preparing an environment-friendly plasticizer by recycling waste resources. The method comprises the following steps of transferring alkali-reduction wastewater containing sodium terephthalate into an acid precipitation tank with a stirring device and adding sulfuric acid to further precipitate terephthalic acid (PTA) solids; carrying out plate-frame filtration on the mixed solution to obtain a crude PTA material; adding the recovered crude PTA material into an esterification reactor with an alcohol-water separation device, adding iso-octanol, heating and dehydrating, adding tetrabutyl titanate as a catalyst and carrying out esterification reaction; after water is no longer produced, stopping reaction and dealcoholizing to obtain a crude DOTP (Dioctyl Terephthalate) product; rectifying the prepared crude DOTP product in a packing-type rectifying tower to obtain a rectified product, adding the rectified product into a neutralization reaction kettle, adding sodium hydroxide lye, stirring and washing with alkali; standing, precipitating and discharging the aqueous solution in the lower layer, adding hot water, stirring and washing with water, standing, precipitating and discharging the moisture in the lower layer, carrying out temperature-raising dehydration, adding an inorganic filter aid and filtering to obtain the pure DOTP product. By the method, the recycling of the waste resources is achieved.

Description

technical field [0001] The invention belongs to the technical field of recycling of waste resources and preparation of plasticizers, and in particular relates to a method for recycling waste resources to prepare environmentally friendly plasticizers. Background technique [0002] In recent years, with the rapid development of my country's polyester fiber industry, alkali reduction treatment technology has been widely used in the production of imitation silk, ultra-fine synthetic leather and other products, resulting in a large amount of alkali reduction wastewater produced every year. The characteristics of wastewater are: high alkalinity, high pollutant content, poor biodegradability, belonging to high-concentration refractory organic wastewater, generally pH>10, COD 1000-80000mg / L. Alkali reduction wastewater contains a large amount of waste resources such as terephthalic acid (existing in the form of sodium salt), fiber degradation by-products, etc. Since PTA is an impo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/82C07C67/08
CPCC07C67/08C07C69/82
Inventor 蒋剑春刘朋陈水根冯国东龚建平徐俊明
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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