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Method for treating high-concentration wastewater in citral synthesis process

A high-concentration wastewater and synthetic process technology, applied in water/sewage treatment, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problems of uneconomical wastewater, long treatment process, poor applicability, etc.

Active Publication Date: 2020-03-31
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above method of wastewater treatment has poor applicability for the treatment of high-concentration wastewater generated by the oxidation of 3-methyl-3-butene-1-ol to 3-methyl-3-butene-1-aldehyde, and the treatment process is long. The cost is high, and it is difficult to realize the reuse of useful substances in wastewater
[0008] Wet oxidation is also an effective method for treating high-concentration organic wastewater. It has high treatment efficiency and rarely causes secondary pollution, but it needs to be carried out under high temperature and high pressure conditions, and catalysts loaded with precious metals are used. The intermediate products are often organic acids. It has a certain poisoning effect and affects the catalytic life. At the same time, it has high requirements for equipment materials, high temperature resistance, high pressure resistance, and corrosion resistance. Therefore, the equipment cost is large and the one-time investment of the system is high; It is carried out under high temperature and high pressure conditions, so it is only suitable for small flow and high concentration wastewater treatment, and it is not economical for high concentration and large volume wastewater
[0009] In view of the shortcomings of the above existing wastewater treatment methods and the characteristics of the high-concentration wastewater generated by the oxidation of 3-methyl-3-butene-1-alcohol to 3-methyl-3-butene-1-aldehyde, it is urgent to develop a method that can An effective treatment method to avoid the impact of wastewater treatment on production, recover organic matter in wastewater, simplify wastewater treatment processes, and reduce production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Preparation of catalyst:

[0066] S1: 3.0541g sodium tetraborate (B 4 h 20 Na 2 o 17 ), 0.3698g sodium tungstate (Na 2 WO 4 2H 2 O) and 2.1228g zirconium nitrate (Zr(NO 3 ) 4 ·5H 2 O) was dissolved in 200g of pure water to obtain a mixed aqueous solution of sodium tetraborate and zirconium nitrate.

[0067] S2: Mix the above mixed aqueous solution with 0.5106g [Pt(NH 3 ) 4 ][PtCl 4 ] mixture, slowly add 151.16g of alumina carrier, fully stir for 20min, add 10wt% dilute hydrochloric acid to adjust the pH to 7, and age at 80°C for 10h. After the above mixed solution was filtered, it was dried at 110°C for 5 hours, after molding, it was calcined at 180°C for 2 hours, and the catalyst was prepared after cooling down.

[0068] Prepared catalyst composition: boron oxide content 0.726wt%, tungsten oxide content 0.169wt%, zirconium oxide content 0.397wt%, [Pt(NH 3 ) 4 ][PtCl 4 ] The content is 0.332wt%, the others are carrier alumina, the content is 98.376%.

...

Embodiment 2

[0074] Preparation of catalyst:

[0075] S1: 0.2885g sodium tetraborate (B 4 h 20 Na 2 o 17 ), 0.0313g sodium tungstate (Na 2 WO 4 2H 2 O) and 0.1206g zirconium nitrate (Zr(NO 3 ) 4 ·5H 2 O) was dissolved in 200g of pure water to obtain a mixed aqueous solution of sodium tetraborate and zirconium nitrate.

[0076] S2: Combine the above mixed aqueous solution with 0.5613g [Pt(NH 3 ) 4 ][PtCl 4 ] into the mixture of 154.6g alumina carrier slowly, fully stirred for 30min, added 10wt% dilute hydrochloric acid to adjust the pH to 5, and aged at 80°C for 20h. After the above mixed solution was filtered, it was dried at 120°C for 3 hours, after molding, it was calcined at 200°C for 4 hours, and the catalyst was prepared after cooling down.

[0077] Prepared catalyst composition: boron oxide content 0.068wt%, tungsten oxide content 0.014wt%, zirconium oxide content 0.022wt%, [Pt(NH 3 ) 4 ][PtCl 4 ] The content is 0.361wt%, the others are carrier alumina, the content is...

Embodiment 3

[0083] Preparation of catalyst:

[0084] S1: 11.473g sodium tetraborate (B 4 h 20 Na 2 o 17 ), 1.521g sodium tungstate (Na 2 WO 4 2H 2 O) and 7.036g zirconium nitrate (Zr(NO 3 ) 4 ·5H 2 O) was dissolved in 400g of pure water to obtain a mixed aqueous solution of sodium tetraborate and zirconium nitrate.

[0085] S2: Combine the above mixed aqueous solution with 0.5317g [Pt(NH 3 ) 4 ][PtBr 4 ] slowly added to 153.73g of vanadium oxide carrier, stirred for 30min, added 5wt% dilute hydrochloric acid to adjust the pH to 6, aged at 70°C for 5h. After the above mixed solution was filtered, it was dried at 110°C for 3 hours, after molding, it was calcined at 250°C for 2 hours, and the catalyst was prepared after cooling down.

[0086] Prepared catalyst composition: boron oxide content 2.593wt%, tungsten oxide content 0.662wt%, zirconium oxide content 1.25wt%, [Pt(NH 3 ) 4 ][PtCl 4 ] with a content of 0.329wt%, and the others are carrier vanadium oxide with a content o...

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Abstract

The invention provides a method for treating high-concentration wastewater in a citral synthesis process. In the method, high-concentration wastewater of 3-methyl-3-butene-1-aldehyde prepared by oxidizing 3-methyl-3-butene-1-alcohol is taken as a raw material, and the method comprises the following steps of: performing stripping to separate alcohol compounds and aldehyde compounds contained in thehigh-concentration wastewater, and converting the high-concentration wastewater into low-concentration wastewater containing acetal compounds; converting the acetal compounds in the low-concentrationwastewater into 3-methyl-3-butene-1 alcohol and 3-methyl-3-butene-1-aldehyde by adopting an acidic hydrolysis reaction, so as to obtain low-concentration wastewater containing hydrolysate; and separating 3-methyl-3-butene-1-alcohol and 3-methyl-3-butene-1-aldehyde from the low-concentration wastewater containing the hydrolysate through stripping, so that the COD of the treated wastewater is reduced to 200 ppm or below. The method is economical and high in treatment efficiency, heavy component impurities are converted into process raw materials and products, and the separation yield is increased.

Description

technical field [0001] The invention belongs to the technical field of sewage treatment, and relates to a treatment method for high-concentration wastewater in the synthesis process of citral, in particular to a method for preparing 3-methyl-3 by oxidation of 3-methyl-3-butene-1-ol in the synthesis process of citral -The treatment method of high-concentration wastewater generated by butene-1-aldehyde. Background technique [0002] Citral is an important chemical raw material with a wide range of uses. It is an important spice for lemon type, deodorant wood type essence, artificially prepared lemon oil, bergamot oil and orange leaf oil. It is the raw material for the synthesis of ionones, vitamin A and methyl ionones. [0003] One of the key reactions in the production of citral by the isobutene method is the oxidation of 3-methyl-3-butene-1-ol to 3-methyl-3-butene-1-aldehyde, and the oxidation reaction products include 3-methyl-3 -butene-1-aldehyde, 3-methyl-2-butene-1-ald...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/10C07C29/09C07C33/025C07C45/51C07C47/21C07C29/80C07C45/82
CPCC02F1/10C02F1/00C07C29/09C07C45/515C07C45/82C07C29/80C02F2101/34C07C33/025C07C47/21
Inventor 朱小瑞张晨李广琼孙钦鹤张鹏举张文立王欢刘英俊沈元伟王文
Owner WANHUA CHEM GRP CO LTD
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