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A kind of treatment method of high concentration wastewater in citral synthesis process

A high-concentration wastewater and synthesis process technology, applied in water/sewage treatment, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problem of affecting catalytic life, high one-time investment, and uneconomical wastewater, etc. problems, to achieve the effect of reducing equipment cost and energy consumption, improving separation yield, and no secondary pollution

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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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 200 g of pure water to obtain a mixed aqueous solution of sodium tetraborate and zirconium nitrate.

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

[0068] The prepared catalyst composition: the content of boron oxide is 0.726wt%, the content of tungsten oxide is 0.169wt%, the content of zirconia is 0.397wt%. 3 ) 4 ][PtCl 4 ] The content is 0.332wt%, the others are carrier alumina, and the content is 98.376%.

[0069] Wastewater trea...

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 200 g of pure water to obtain a mixed aqueous solution of sodium tetraborate and zirconium nitrate.

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

[0077] The prepared catalyst composition: the content of boron oxide is 0.068wt%, the content of tungsten oxide is 0.014wt%, the content of zirconia is 0.022wt%. 3 ) 4 ][PtCl 4 ] The content is 0.361wt%, the others are carrier alumina, and the content is 99.534%.

[0078] Wast...

Embodiment 3

[0083] Preparation of catalyst:

[0084] S1: 11.473 g of 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 400 g of pure water to obtain a mixed aqueous solution of sodium tetraborate and zirconium nitrate.

[0085] S2: mix the above mixed aqueous solution with 0.5317 g [Pt(NH 3 ) 4 ][PtBr 4 ] was slowly added to 153.73 g of vanadium oxide carrier, stirred for 30 min, adjusted to pH 6 by adding 5 wt% dilute hydrochloric acid, and aged at 70° C. for 5 h. The above mixture was filtered, dried at 110 °C for 3 hours, calcined at 250 °C for 2 hours after molding, and cooled to obtain a catalyst.

[0086] The prepared catalyst composition: the content of boron oxide is 2.593wt%, the content of tungsten oxide is 0.662wt%, the content of zirconia is 1.25wt%. 3 ) 4 ][PtCl 4 ] The content is 0.329wt%, the others are carrier vanadium oxide, and the content is 95.166%. ...

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Abstract

The invention provides a method for treating high-concentration wastewater in a citral synthesis process. Using high-concentration wastewater obtained by oxidizing 3-methyl-3-butene-1-alcohol to prepare 3-methyl-3-butene-1-aldehyde as a raw material, the steps include: stripping and separating alcohols contained in the high-concentration wastewater compound and aldehyde compounds, converting high-concentration wastewater into low-concentration wastewater containing acetal compounds; converting the acetal compounds in the low-concentration wastewater into 3-methyl-3-butene-1 alcohol and 3-methyl-3-butene-1-aldehyde, to obtain low-concentration waste water containing hydrolyzate; Separating the low-concentration waste water containing hydrolyzate by stripping 3-methyl-3-butene-1 alcohol and 3-methyl base-3-butene-1-aldehyde, reducing the COD of the treated wastewater to below 200ppm. The method is economical, has high processing efficiency, and converts heavy component impurities into process raw materials and products, thereby improving the separation yield.

Description

technical field [0001] The invention belongs to the technical field of sewage treatment, relates to a method for treating high-concentration wastewater in a citral synthesis process, and in particular relates to a kind of oxidation of 3-methyl-3-buten-1-ol to 3-methyl-3 in a citral synthesis process -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 formulated lemon oil, bergamot oil and orange leaf oil. It is the raw material for synthesizing ionone, vitamin A and methyl ionone. [0003] One of the key reactions in the production of citral by isobutene is the oxidation of 3-methyl-3-buten-1-ol to 3-methyl-3-butene-1-aldehyde. The oxidation reaction products include 3-methyl-3 -Butene-1-aldehyde, 3-methyl-2-butene-1-aldehyde and water, the reaction solutio...

Claims

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Application Information

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Patent Type & Authority Patents(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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