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Method for Improving the Quality of Adiponitrile

A technology of adiponitrile and impurities, applied in the field of improving the quality of adiponitrile

Active Publication Date: 2015-08-12
INVISTA TEXTILES (U K) LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] However, there remains a need for improved methods of using ozone to reduce or eliminate the problems associated with impurities in ADN

Method used

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  • Method for Improving the Quality of Adiponitrile
  • Method for Improving the Quality of Adiponitrile
  • Method for Improving the Quality of Adiponitrile

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Air was passed through a Wedeco ozone generator, Model SMA 500S, at a rate of 30 Nm3 / hr to produce an ozone concentration of 1.0% by weight in the air. An ozone-containing air stream is fed to the PFSMR along with a refined adiponitrile stream. The adiponitrile feed rate was 13.2 metric tons / hour. The static mixer included Sulzer SMV elements. There are a total of six mixing sections, and each section is 6 feet (1.8 m) long, providing a total static mixer length of 36 feet (11 m). Each 6-foot (1.8-m) long segment includes six static mixer elements, each of which is 6 inches (15.2 cm) long, wherein each of the elements passes through a 6-inch (15.2 cm) opening Tubes, ie pipes without static mixer elements, are separated from each other. The diameter of the static mixer is 3 inches (7.6 cm). Based on the measured properties, the mass transfer parameter k L a is calculated to be about 0.7 seconds -1 . The adiponitrile feed contained 5.7 ppm phosphorus in the form of...

Embodiment 2

[0040] This example shows the improved ozone utilization achieved by performing the reaction in a plug flow reactor (PFR) relative to a back-mix reactor (CSTR). This example is a computer simulation of a process based on a conventional reactor selectivity model using experimentally determined data on the relative reaction rates of various impurities with ozone. In this example, the ADN feed to the two simulated reactors contained the following impurities: 10 ppm of P(III), 50 ppm of CPI, 25 ppm of TBC and 675 ppm of DDN.

[0041] The reaction stoichiometry for the reaction of ozone with the impurities present is 1 mole of ozone each per mole of P(III), CPI and DDN; for TBC, the stoichiometry is 3 moles of ozone per mole of TBC. Experiments were performed in which refined ADN was reacted with ozone in a CSTR at atmospheric pressure and ambient temperature. Depletion of P(III), CPI, TBC and DDN in CSTR was measured. These data were fitted to a CSTR reactor design model derived...

Embodiment 3

[0042] This example shows the beneficial effect of reducing HMI yield during HMD production by treating ADN with ozone to destroy TBC prior to hydrogenation.

[0043] 1 part by weight of ADN was continuously mixed with 6 parts by weight of anhydrous ammonia. This mixture is fed to a bed of heterogeneous iron catalyst together with a stoichiometric excess of hydrogen. The stoichiometric amount of hydrogen is 4 moles of hydrogen per mole of ADN. The reactor was operated at a pressure of about 5000 psi (34.5 MPa). The reactor feed temperature is about 100°C and the temperature increases along the length of the bed due to the heat of reaction of ADN with hydrogen.

[0044] Initially, ozonated ADN was fed to the reactor for a period of 250 hours. The conversion yield from ADN to HMI averaged 0.10% (moles of HMI formed per mole of ADN reacted x 100%) over this time period when the ozonated ADN was fed to the reactor. The ADN feed was then converted to unozone-treated ADN and run...

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Abstract

A process and apparatus for reacting deleterious impurities contained in adiponitrile (ADN) comprises feeding ADN and an ozone containing gas into a co-current plug flow reactor containing static mixer elements, to oxidize at least a portion of the impurities, thereby producing a reactor discharge, which is processed to produce an ozone-treated ADN product.

Description

Area of invention [0001] The present invention involves methods and devices for improving the quality of 二 腈 (ADN).The present invention specially involves ozone treatment of ADN to respond to the impurities reactions (or remove such impurities from the ADN) with the harmful marks in ADN.The hydrogenation of amino (ACN) and hexalomyramine (HMD) has adverse effects. Background technique [0002] It is known that nylon 66 can be prepared in multi -step methods.In the first step, the bonotenhyl (BD) hydrogen cyanocyrosis was used under the existence of a hydrogen cyanide (HCN) to prepare the two pupa (ADN).Subsequently, organic impurities were removed from ADN to prepare refined ADN.The appropriate method used to remove organic impurities includes extraction and distillation.See Ostermaier's US patent 6,331,651, the US patent is combined here by reference.In the next step, the refined ADN catalyzes hydrogenation to prepare HMD or a mixture containing ACN and HMD.Appropriate hydride ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/34B01D3/40C07C255/04
CPCC07C253/34C07C255/04
Inventor 约翰·J·奥斯特麦尔布鲁斯·E·默弗里
Owner INVISTA TEXTILES (U K) LTD
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