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Method for treating waste liquid generated in polyolefin catalyst production, obtained titanium tetraalkoxide and application thereof

A technology of polyolefin catalyst and tetraalkoxytitanium, which is applied in the field of waste liquid reuse, can solve the problems of time-consuming, difficult to scale up and implement equipment costs, and high energy consumption, and achieve the effect of cheap chemicals

Active Publication Date: 2021-02-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this technology is difficult to scale up due to the cost of equipment
CN101717113A adopts the method of cold precipitation and precipitation to avoid coking, but the operation needs to be operated below 0°C, which consumes a lot of energy and takes a long time

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] A 500 ml three-necked flask was placed in an ice-water bath, magnetically stirred, protected by nitrogen, connected to a tail gas absorbing device, and contained 20% aqueous sodium hydroxide solution in the tail gas absorbing bottle. Add 35 grams of waste liquid (all the rest are toluene) produced by the production Ziegler-Natta catalyst that contains 25% titanium tetrachloride, slowly drip the ethanol solution (2 moles per liter) of ammonia with constant pressure funnel 150 Milliliters, control reaction temperature during dropwise addition and be no more than 25 degrees Celsius. After the dropwise addition was completed, the reaction was carried out for 4 hours. stand still. Under the condition of isolation of water and oxygen, filter to obtain white powder and light yellow clear liquid. The weight of the white powder was 9.1 g after drying; the light yellow clear liquid was distilled under reduced pressure to obtain 10.2 g of yellow liquid (titanium tetraethoxide). ...

Embodiment 2

[0060] 250 milliliter three-neck flask, magnetic stirring, nitrogen protection, add 61.3 grams of No. 1 waste liquid (the content of titanium tetrachloride is relatively high, in addition contains toluene and organophosphorus compound), under 70 ℃ absolute pressure 80mbar vacuum distillation, separate most 46.9 grams of solvent and part of titanium tetrachloride, 14.4 grams of residual waste liquid;

[0061] 250 milliliters of three-necked flasks, magnetic stirring, nitrogen protection, add No. 2 waste liquid (titanium tetrachloride content is low, contain hexane, toluene and organophosphorus compound) 45.0 grams, absolute pressure 80mbar vacuum distillation under 70 ℃, separate 41.0 grams of most solvents and part of titanium tetrachloride, 5.0 grams of residual waste liquid;

[0062] Combine the residual waste liquid of No. 1 waste liquid and No. 2 waste liquid into a 1000 ml three-necked flask, place it in an ice-water bath, stir it magnetically, protect it with nitrogen, c...

Embodiment 3

[0064] Repeat the process of Example 1, the difference is that a four-necked flask is used, and the ethanol solution of ammonia is added dropwise to the waste liquid at two symmetrical openings on the four-necked flask. At the same time, the two drops are staggered and not carried out at the same time.

[0065] Under such a dropping system, it is found that the ethanol solution of ammonia can be added dropwise earlier, and a high recovery rate is also obtained.

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PUM

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Abstract

The invention relates to a method for treating waste liquid generated in polyolefin catalyst production, obtained titanium tetraalkoxide and application thereof. The method comprises the following steps: 1, mixing ammonia and / or amine with an alcohol compound, and obtaining an alcohol solution of ammonia and / or amine; step 2, adding an alcoholic solution of ammonia and / or amine into the waste liquid; 3, carrying out solid-liquid separation, and taking a liquid phase; and 4, distilling the liquid phase, and recycling the distilled alcohol compound to obtain the titanium tetraalkoxide; and optionally carrying out step 2' before the step 2: carrying out distillation treatment on the waste liquid, separating out an organic solution of titanium tetrachloride, and obtaining a distillation residual liquid. By adopting the method disclosed by the invention, the titanium tetrachloride contained in the waste liquid generated in the production of the Ziegler-Natta catalyst can be efficiently, completely and safely converted into the tetraalkoxy titanium, and no secondary waste liquid is generated in the reaction process.

Description

technical field [0001] The invention relates to the reuse of waste liquid, in particular to the treatment of waste liquid containing titanium compounds, in particular to a method for treating waste liquid produced in the production of polyolefin catalysts, obtained tetraalkoxy titanium and applications thereof. Background technique [0002] Polyolefin is the largest synthetic material in the world, with an annual output of nearly 200 million tons. The catalysts currently used in the production of polyolefins are mainly Ziegler-Natta catalysts. The production of Ziegler-Natta catalyst is to load titanium tetrachloride on the carrier, the carrier is mainly magnesium compound, such as magnesium chloride, and some organic matter is added as electron donor during the loading process to improve the polymerization performance of the catalyst. During the production of Ziegler-Natta catalysts, a large amount of waste liquid will be produced, which contains a large amount of titanium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/28C09D7/63C08K5/00
CPCC07F7/003C09D7/63C08K5/0091
Inventor 王伟王洪涛张韬毅
Owner CHINA PETROLEUM & CHEM CORP
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