CN105251481A - Preparation method of dechlorination catalyst - Google Patents
Preparation method of dechlorination catalyst Download PDFInfo
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- CN105251481A CN105251481A CN201510776097.XA CN201510776097A CN105251481A CN 105251481 A CN105251481 A CN 105251481A CN 201510776097 A CN201510776097 A CN 201510776097A CN 105251481 A CN105251481 A CN 105251481A
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- sodium metasilicate
- dechlorination catalyst
- palladium
- aluminium
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Abstract
The invention discloses a preparation method of a dechlorination catalyst. The dechlorination catalyst is obtained in the mode that sodium metasilicate and a metal source react under the environment of an organic phase. Compared with the prior art, the dechlorination catalyst is used for dispersing and fixing palladium and aluminum which have a catalytic effect to a silica gel carrier, and the contact area between the dechlorination catalyst and reaction bed charge is increased. Compared with the prior art, the catalytic efficiency of the dechlorination catalyst is higher, the needed catalytic condition is more moderate, and industrial production is facilitated. Meanwhile, the method is completed under the condition of a pure organic phase, and according to comparison with the common water containing condition, and the catalytic efficiency of the obtained dechlorination catalyst is higher.
Description
Technical field
The invention belongs to catalyst field, be specifically related to a kind of preparation method of dechlorination catalyst.
Background technology
The low-carbon alkene such as ethene, propylene is raw material the most basic in petrochemical industry.For ethene, about there are the petrochemicals of 75% by ethylene production, it is mainly used to produce the multiple important Organic chemical products such as polyethylene, polyvinyl chloride, ethylene oxide/ethylene glycol, dichloroethanes, styrene, polystyrene, ethanol, vinyl acetate, in fact, ethylene yield has become the mark of a measurement national oil chemical engineering industry development level.
Statistics display, from nineteen ninety by 2003, China's ethene equivalent consumption figure increases by 12% every year, after this growth rate is more surprising, within 2003, China's ethene equivalent consumption figure is 1,350 ten thousand tons, within 2005, this numeral just reaches 1,876 ten thousand tons, has increased nearly 40% on foot between 2 years, and Chinese Market for Ethylene has become the country that global growth rate is the fastest, the growth duration is the longest.
In preparing ethylene, propylene and subsequent technique thereof, the effect of dechlorination catalyst has great impact for the productive rate of product and qualification rate.Raney's nickel is a kind of common, efficient dechlorination catalyst, but its preparation cost is higher.Therefore, a kind of efficient, the two series catalysts of nickel aluminium of low cost is a current large study hotspot.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of dechlorination catalyst, not high to solve the catalytic efficiency of prior art existence, the problems such as catalytic condition is harsh.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
A preparation method for dechlorination catalyst, it comprises the steps:
(1) sodium metasilicate is dissolved in organic solvent, under the condition of nitrogen protection, in organic solvent, passes into hydrogen chloride gas, at 20 ~ 50 DEG C, react 2 ~ 4h;
(2) keep nitrogen protection condition, in the mixed system of step (1) gained, add copper source, at 60 ~ 80 DEG C, react 2 ~ 6h;
(3) in the mixed system of gained in step (2), add precipitating reagent, fully mix, after colloidal sol is complete, get gel;
(4) by after the gel detergent of gained in step (3), drying, roast, dechlorination catalyst is obtained.
Wherein, described sodium metasilicate is anhydrous sodium metasilicate.
Wherein, in above-mentioned preparation method, in step (1) ~ (3), agents useful for same is all through anhydrous process.
Wherein, in above-mentioned preparation method, in step (1) and (2), reaction is all placed on shaking table to be carried out.
In step (1), described organic solvent is pyridine or methyl-sulfoxide.
In step (1), the weight ratio of sodium metasilicate and organic solvent is 1:200 ~ 400.
In step (1), the mol ratio of sodium metasilicate and hydrogen chloride is 1:3 ~ 5.
In step (2), described source metal is palladium source and aluminium source; Wherein, palladium source is palladium nitrate, and aluminium source is aluminium chloride.
In step (2), in sodium metasilicate and palladium nitrate, the mol ratio of palladium is 60 ~ 67:1, and in sodium metasilicate and aluminium chloride, the mol ratio of aluminium is 70 ~ 95:1.
In step (3), described precipitating reagent is polyacrylamide or ferric sulfate; Wherein, the mass ratio of precipitating reagent and sodium metasilicate is 1:400 ~ 620.
In step (4), the method for washing is for using deionized water rinsing 2 ~ 3 times, and dry method is for using sodium sulfite dry, and the method for roast is roasting 1 ~ 3h at 700 ~ 800 DEG C.
The dechlorination catalyst that above-mentioned preparation method prepares is also within protection scope of the present invention.
Above-mentioned dechlorination catalyst in the application of catalyst field also within protection scope of the present invention.
Beneficial effect: compared with prior art, the present invention has following advantage:
Dechlorination catalyst in the present invention, is fixed on silica-gel carrier by the palladium and aluminium dispersion that play catalytic action, expands itself and the contact area of reacting bed material.Compared with prior art, this dechlorination catalyst can provide two kinds of catalytic metals simultaneously, and catalytic efficiency is higher, and required catalytic condition milder, is conducive to industrial production.Meanwhile, the inventive method completes under pure organic phase condition, and through contrast, more general aqueous conditions, gained dechlorination catalyst catalytic efficiency is higher.
Detailed description of the invention
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
The preparation of embodiment 1 catalyst
Preparation method:
(1) anhydrous sodium metasilicate is dissolved in methyl-sulfoxide, under the condition of nitrogen protection, in methyl-sulfoxide, passes into hydrogen chloride gas, on shaking table, react 3h at 40 DEG C;
(2) keep nitrogen protection condition, in the mixed system of step (1) gained, add palladium nitrate and aluminium chloride, on shaking table, react 5h at 75 DEG C;
(3) in the mixed system of gained in step (2), add polyacrylamide, fully mix, after colloidal sol is complete, get gel;
(4) by the gel of gained in step (3) with after deionized water rinsing 2 ~ 3 times, dry with sodium sulfite, finally at 750 DEG C, after roasting 2h, obtain dechlorination catalyst.
In step (1) ~ (3), agents useful for same is all through anhydrous process.
In step (1), the weight ratio of anhydrous sodium metasilicate and organic solvent is 1:380.
In step (1), the mol ratio of anhydrous sodium metasilicate and hydrogen chloride is 1:4.
In step (2), in anhydrous sodium metasilicate and palladium nitrate, the mol ratio of palladium is 65:1, and in anhydrous sodium metasilicate and aluminium chloride, the mol ratio of aluminium is 82:1.
In step (3), the mass ratio of polyacrylamide and anhydrous sodium metasilicate is 1:520.
Comparative example 1
Preparation method is with embodiment 1, and difference is, sodium metasilicate used is metasilicate pentahydrate sodium.
Comparative example 2
Preparation method is with embodiment 1, and difference is, methyl-sulfoxide is replaced with water.
Embodiment 2
The dechlorination catalyst prepared in embodiment 1, comparative example 1 and comparative example 2 is used in the reaction of the dealuminated USY cataluyst of 3-chlorophenol.According to the conversion of reaction rate, if the catalytic efficiency of dechlorination catalyst is 1 in embodiment 1, the catalytic efficiency in comparative example 1 is 0.82, and the catalytic efficiency in comparative example 2 is 0.67.
Embodiment 3
By the dechlorination catalyst for preparing in embodiment 1 and existing palladium Al catalysts (by document " palladium/Al bimetal system is to the dealuminated USY cataluyst of 3-chlorophenol " (" environmental project journal ", 2012,2nd phase: 381-384)) in method prepare) in reaction for the dealuminated USY cataluyst of 3-chlorophenol.According to the conversion of reaction rate, if the catalytic efficiency of dechlorination catalyst is 1 in embodiment 1, the catalytic efficiency of commercially available Raney's nickel is 0.79.
Claims (8)
1. a preparation method for dechlorination catalyst, is characterized in that, comprises the steps:
(1) sodium metasilicate is dissolved in organic solvent, under the condition of nitrogen protection, in organic solvent, passes into hydrogen chloride gas, at 20 ~ 50 DEG C, react 2 ~ 4h;
(2) keep nitrogen protection condition, in the mixed system of step (1) gained, add source metal, at 60 ~ 80 DEG C, react 2 ~ 6h;
(3) in the mixed system of gained in step (2), add precipitating reagent, fully mix, after colloidal sol is complete, get gel;
(4) by after the gel detergent of gained in step (3), drying, roast, dechlorination catalyst is obtained.
2. preparation method according to claim 1, is characterized in that, in step (1), described organic solvent is pyridine or methyl-sulfoxide.
3. preparation method according to claim 1, is characterized in that, in step (1), the weight ratio of sodium metasilicate and organic solvent is 1:200 ~ 400.
4. preparation method according to claim 1, is characterized in that, in step (1), the mol ratio of sodium metasilicate and hydrogen chloride is 1:3 ~ 5.
5. preparation method according to claim 1, is characterized in that, in step (2), described source metal is palladium source and aluminium source; Wherein, palladium source is palladium nitrate, and aluminium source is aluminium chloride.
6. the preparation method according to claim 1 and 5, is characterized in that, in step (2), in sodium metasilicate and palladium nitrate, the mol ratio of palladium is 60 ~ 67:1, and in sodium metasilicate and aluminium chloride, the mol ratio of aluminium is 70 ~ 95:1.
7. preparation method according to claim 1, is characterized in that, in step (3), described precipitating reagent is polyacrylamide or ferric sulfate; Wherein, the mass ratio of precipitating reagent and sodium metasilicate is 1:400 ~ 620.
8. preparation method according to claim 1, is characterized in that, in step (4), the method for washing is for using deionized water rinsing 2 ~ 3 times, and dry method is for using sodium sulfite dry, and the method for roast is roasting 1 ~ 3h at 700 ~ 800 DEG C.
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| CN201510776097.XA CN105251481A (en) | 2015-11-13 | 2015-11-13 | Preparation method of dechlorination catalyst |
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| CN201510776097.XA CN105251481A (en) | 2015-11-13 | 2015-11-13 | Preparation method of dechlorination catalyst |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731570A (en) * | 2018-12-17 | 2019-05-10 | 嘉兴学院 | It is a kind of for detecting the loaded palladium catalyst preparation method of short chain chlorinated paraffin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4749817A (en) * | 1986-08-22 | 1988-06-07 | Standard Chlorine Of Delaware, Inc. | Hydrodechlorination of chlorinated benzenes |
| CN103633268A (en) * | 2012-08-22 | 2014-03-12 | 海洋王照明科技股份有限公司 | Preparation method of silicon dioxide composite separators |
| CN104190396A (en) * | 2014-08-28 | 2014-12-10 | 无锡普爱德环保科技有限公司 | Preparation method of lithium-loaded silica gel catalyst |
-
2015
- 2015-11-13 CN CN201510776097.XA patent/CN105251481A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4749817A (en) * | 1986-08-22 | 1988-06-07 | Standard Chlorine Of Delaware, Inc. | Hydrodechlorination of chlorinated benzenes |
| CN103633268A (en) * | 2012-08-22 | 2014-03-12 | 海洋王照明科技股份有限公司 | Preparation method of silicon dioxide composite separators |
| CN104190396A (en) * | 2014-08-28 | 2014-12-10 | 无锡普爱德环保科技有限公司 | Preparation method of lithium-loaded silica gel catalyst |
Non-Patent Citations (4)
| Title |
|---|
| 卢勇宏，等: "纳米钯/铝双金属对水中3-氯酚的脱氯降解研究", 《环境污染与防治》 * |
| 朱洪法: "《催化剂载体制备及应用技术》", 31 October 2014, 石油工业出版社 * |
| 杨波，等: "钯/铝双金属体系对3-氯酚的脱氯降解", 《环境工程学报》 * |
| 陆鼎一: "《化学故事新编》", 31 July 2007, 苏州大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731570A (en) * | 2018-12-17 | 2019-05-10 | 嘉兴学院 | It is a kind of for detecting the loaded palladium catalyst preparation method of short chain chlorinated paraffin |
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Application publication date: 20160120 |
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