CN110368947A - A kind of preparation method of dimethyl maleate hydrogenation catalyst - Google Patents
A kind of preparation method of dimethyl maleate hydrogenation catalyst Download PDFInfo
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- CN110368947A CN110368947A CN201910735530.3A CN201910735530A CN110368947A CN 110368947 A CN110368947 A CN 110368947A CN 201910735530 A CN201910735530 A CN 201910735530A CN 110368947 A CN110368947 A CN 110368947A
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- catalyst
- dimethyl maleate
- warming
- adds hydrogen
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/30—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group
- C07C67/303—Preparation of carboxylic acid esters by modifying the acid moiety of the ester, such modification not being an introduction of an ester group by hydrogenation of unsaturated carbon-to-carbon bonds
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Abstract
The invention discloses the method for preparing catalyst that a kind of dimethyl maleate adds hydrogen, the aqueous solution of nickel nitrate and ammonium hydroxide react at a certain temperature first is precipitated, it is dried after filtering washing, product and light aluminum oxide mixing after drying, it is mediated by kneader, granulating roasting after kneading, obtains catalyst prod.For the catalyst that the present invention obtains while guaranteeing activity, catalysis time is long, and the catalyst relative to addition noble metal is low in cost, and the preparation method of catalyst is simple and easy to get.
Description
Technical field
The invention belongs to chemical technology fields, and in particular to a kind of preparation method of dimethyl maleate hydrogenation catalyst.
Background technique
The synthetic perfume and food additives that dimethyl succinate is important, can be used as food antiseptics, are mainly used for
Prepare fruit and fruit wine class essence.For pharmaceuticals industry, synthesis light stabilizer, high-grade paint, fungicide, medicine intermediate, conjunction
At light stabilizer, high-grade paint, fungicide, medicine intermediate etc..Principal synthetic route is methanol and succinic acid urging in sulfuric acid
It is reacted to obtain under change, requirement of this method to equipment is high, and the corrosivity of sulfuric acid is strong, and there are certain risk, and
Pollute environment.What existing dimethyl maleate and hydrogen reacted under the effect of the catalyst arrives product.This method is easy to operate,
It is suitble to large-scale production.The hydrotalcite of the nickel class of patent CN 103657693 does carrier, by supporting palladium nitrate, then loads it
Remaining microelement prepares catalyst, and catalyst cost is relatively high.
Summary of the invention
To solve the above problems, the present invention provides the catalyst that a kind of dimethyl maleate adds hydrogen, making for noble metal is reduced
While to reduce catalyst cost, higher activity is still able to maintain after long period of operation, preparation method is simple and easy to get.
The invention is realized by the following technical scheme:
Catalyst provided by the invention is reacted with nickel nitrate aqueous solution and ammonium hydroxide at a certain temperature first to be precipitated, mistake
Drainage is dried after washing, and product and light aluminum oxide mixing after drying are mediated, granulating roasting after kneading is obtained by kneader
Catalyst prod.
1) 60%-70% nickel nitrate aqueous solution, is prepared, aqueous solution is added in reaction kettle, certain temperature is warming up to；
2) 25-28wt% ammonium hydroxide is added dropwise after, reaching temperature, is stirred 1 hour after being added dropwise, cooling filtering washing；
3), that the product after washing is dry in 100 DEG C of thermostatic drying chambers, obtain complex；
4), the product after a certain amount of water, light aluminum oxide and drying is added portionwise in kneader and is mediated, is made after kneading
Grain；
5) catalyst after, being granulated obtains dimethyl maleate hydrogenation catalyst by roasting.
In the above-mentioned technical solutions, nickel nitrate is six water nickel nitrates in step 1, and reaction temperature is 60-70 DEG C.
In the above-mentioned technical solutions, the mass ratio of ammonia spirit and nickel nitrate aqueous solution is preferably 1:1.5-2 in step 2.
In the above-mentioned technical solutions, product, light aluminum oxide and the water three's mass ratio in step 4 after drying are preferably
1:1-1.5:3.5-4。
In the above-mentioned technical solutions, the dosage of washing water is 3 times of dosage of 25-28wt% ammonium hydroxide, is washed to solid precipitating
Object is not being reduced.
In the above-mentioned technical solutions, calcination procedure is to keep the temperature 120min after 3.5 DEG C/min is warming up to 200 DEG C in step 5,
350 DEG C of heat preservation 120min are warming up to 2.5 DEG C/min again, then 600 DEG C of heat preservation 360min are warming up to 2 DEG C/min, after cooling
To finished catalyst.
Specific embodiment
Embodiment 1
It takes 1407g nickel nitrate and 2100g water dissolution is mixed to obtain 67% nickel nitrate aqueous solution to pour into reaction kettle
It is warming up to 65 DEG C, 27% ammonium hydroxide 800g is added dropwise, 1h is added dropwise, is cooled to room temperature filtering after stirring 1h, takes 2400g moisture three times
Washing, dries in 100 DEG C of constant temperature ovens of product after washing, obtains product 290g.Weigh light aluminum oxide that 386g is not burnt and
1080g water is mediated in kneader after mixing, and the catalyst being granulated is roasted according to the temperature program of roasting, obtains Malaysia
Dimethyl phthalate hydrogenation catalyst.It takes 4g Catalyst packing in fixed bed, is warming up to 190 DEG C, hydrogen flowing quantity 200ml/min, horse
Carrying out dimethyl phthalate air speed is 0.5h-1, feed stock conversion is dimethyl maleate 98.45%, product dimethyl succinate selectivity
93.86%.
Embodiment 2
It takes 1280g nickel nitrate and 2100g water dissolution is mixed to obtain 61% nickel nitrate aqueous solution to pour into reaction kettle
It is warming up to 65 DEG C, 27% ammonium hydroxide 857g is added dropwise, 1h is added dropwise, is cooled to room temperature filtering after stirring 1h, takes 2400g moisture three times
Washing, dries in 100 DEG C of constant temperature ovens of product after washing, obtains product 275g.Weigh light aluminum oxide that 366g is not burnt and
1030g water is mediated in kneader after mixing, and the catalyst being granulated is roasted according to the temperature program of roasting, obtains Malaysia
Dimethyl phthalate hydrogenation catalyst.It takes 4g Catalyst packing in fixed bed, is warming up to 190 DEG C, hydrogen flowing quantity 200ml/min, horse
Carrying out dimethyl phthalate air speed is 0.5h-1, feed stock conversion 98.68%, selectivity of product 93.80%.
Embodiment 3
It takes 1365g nickel nitrate and 2100g water dissolution is mixed to obtain 65% nickel nitrate aqueous solution to pour into reaction kettle
It is warming up to 65 DEG C, 27% ammonium hydroxide 685g is added dropwise, 1h is added dropwise, is cooled to room temperature filtering after stirring 1h, takes 2400g moisture three times
Washing, dries in 100 DEG C of constant temperature ovens of product after washing, obtains product 277g.Weigh light aluminum oxide that 355g is not burnt and
1008g water is mediated in kneader after mixing, and the catalyst being granulated is roasted according to the temperature program of roasting, obtains Malaysia
Dimethyl phthalate hydrogenation catalyst.It takes 4g Catalyst packing in fixed bed, is warming up to 190 DEG C, hydrogen flowing quantity 200ml/min, horse
Carrying out dimethyl phthalate air speed is 0.5h-1, feed stock conversion 98.60%, selectivity of product 93.60%.
Embodiment 4
It takes 1400g nickel nitrate and 2100g water dissolution is mixed to obtain 67% nickel nitrate aqueous solution to pour into reaction kettle
It is warming up to 65 DEG C, 27% ammonium hydroxide 800g is added dropwise, 1h is added dropwise, is cooled to room temperature filtering after stirring 1h, takes 2400g moisture three times
Washing, dries in 100 DEG C of constant temperature ovens of product after washing, obtains product 290g.Weigh light aluminum oxide that 580g is not burnt and
1220g water is mediated in kneader after mixing, and the catalyst being granulated is roasted according to the temperature program of roasting, obtains Malaysia
Dimethyl phthalate hydrogenation catalyst.It takes 4g Catalyst packing in fixed bed, is warming up to 190 DEG C, hydrogen flowing quantity 200ml/min, horse
Carrying out dimethyl phthalate air speed is 0.5h-1, feed stock conversion 97.0%, selectivity of product 94.0%.
Embodiment 5
It takes 1400g nickel nitrate and 2100g water dissolution is mixed to obtain 67% nickel nitrate aqueous solution to pour into reaction kettle
It is warming up to 65 DEG C, 27% ammonium hydroxide 800g is added dropwise, 1h is added dropwise, is cooled to room temperature filtering after stirring 1h, takes 2400g moisture three times
Washing, dries in 100 DEG C of constant temperature ovens of product after washing, obtains product 290g.Weigh light aluminum oxide that 350g is not burnt and
1020g water is mediated in kneader after mixing, and the catalyst being granulated is roasted according to the temperature program of roasting, obtains Malaysia
Dimethyl phthalate hydrogenation catalyst.It takes 4g Catalyst packing in fixed bed, is warming up to 190 DEG C, hydrogen flowing quantity 200ml/min, horse
Carrying out dimethyl phthalate air speed is 0.5h-1, feed stock conversion 98.7%, selectivity of product 93.80%.
Claims (6)
1. the method for preparing catalyst that a kind of dimethyl maleate adds hydrogen, which is characterized in that this method comprises the following steps:
Step 1: 60wt%-70wt% nickel nitrate aqueous solution is prepared, aqueous solution is added in reaction kettle, certain temperature is warming up to
Degree；
Step 2: being added dropwise 25-28wt% ammonium hydroxide after reaching temperature, stir 1 hour after being added dropwise, cooling filtering washing；
Step 3: the product after washing is dry in 100 DEG C of -120 DEG C of thermostatic drying chambers, obtain complex；
Step 4: the product after will be dry in a certain amount of water, light aluminum oxide and step 3, which is added portionwise in kneader, to be mediated,
It is granulated after kneading；
Step 5: the catalyst after granulation obtains dimethyl maleate hydrogenation catalyst by roasting.
2. the method for preparing catalyst that dimethyl maleate according to claim 1 adds hydrogen, it is characterised in that: in step 1
Nickel nitrate is six water nickel nitrates.
3. the method for preparing catalyst that dimethyl maleate according to claim 1 adds hydrogen, it is characterised in that: in step 1
It is warming up to 60-70 DEG C.
4. the method for preparing catalyst that dimethyl maleate according to claim 1 adds hydrogen, it is characterised in that: in step 2
The mass ratio of ammonia spirit and nickel nitrate is 1:1.5-2.5.
5. the method for preparing catalyst that dimethyl maleate according to claim 1 adds hydrogen, it is characterised in that: in step 4
Product, light aluminum oxide and water three's mass ratio after drying are 1:1-2:3.5-4.5.
6. the method for preparing catalyst that dimethyl maleate according to claim 1 adds hydrogen, it is characterised in that: in step 5
Calcination procedure is to keep the temperature 120min after 3.5 DEG C/min is warming up to 200 DEG C, then be warming up to 350 DEG C of heat preservations with 2.5 DEG C/min
120min, then 600 DEG C of heat preservation 360min are warming up to 2 DEG C/min, finished catalyst is obtained after cooling.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112973697A (en) * | 2021-03-01 | 2021-06-18 | 广东工业大学 | Catalyst for hydrogenation reaction and synthesis method for catalyzing fatty acid methyl ester by using catalyst |
Citations (8)
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|---|---|---|---|---|
| US3950441A (en) * | 1970-09-16 | 1976-04-13 | Gaf Corporation | Process and catalyst for preparing 1,4-butanediol |
| JPH0268142A (en) * | 1988-08-31 | 1990-03-07 | Agency Of Ind Science & Technol | Hydrogenation catalyst and its preparation |
| CN101891714A (en) * | 2010-08-12 | 2010-11-24 | 湖南长岭石化科技开发有限公司 | Method for producing tetrahydrofuran |
| CN101927166A (en) * | 2010-07-23 | 2010-12-29 | 南京大学 | Nickel-carried catalyst as well as preparation method and application thereof |
| CN101979139A (en) * | 2010-10-26 | 2011-02-23 | 中国科学院山西煤炭化学研究所 | Catalyst of succinic acid dicarboxylic ester and preparation method thereof |
| CN103769094A (en) * | 2014-01-20 | 2014-05-07 | 中国科学院宁波材料技术与工程研究所 | Eggshell type catalyst for selective hydrogenation reaction as well as preparation method and application thereof |
| CN104399468A (en) * | 2014-11-24 | 2015-03-11 | 南京工业大学 | Nickel-based catalyst, and preparation method and application thereof |
| CN110078617A (en) * | 2019-05-14 | 2019-08-02 | 常州大学 | A method of cyclohexane cyclohexanedimethanodibasic ester is prepared with phthalic acid ester catalytic hydrogenation |
-
2019
- 2019-08-09 CN CN201910735530.3A patent/CN110368947A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3950441A (en) * | 1970-09-16 | 1976-04-13 | Gaf Corporation | Process and catalyst for preparing 1,4-butanediol |
| JPH0268142A (en) * | 1988-08-31 | 1990-03-07 | Agency Of Ind Science & Technol | Hydrogenation catalyst and its preparation |
| CN101927166A (en) * | 2010-07-23 | 2010-12-29 | 南京大学 | Nickel-carried catalyst as well as preparation method and application thereof |
| CN101891714A (en) * | 2010-08-12 | 2010-11-24 | 湖南长岭石化科技开发有限公司 | Method for producing tetrahydrofuran |
| CN101979139A (en) * | 2010-10-26 | 2011-02-23 | 中国科学院山西煤炭化学研究所 | Catalyst of succinic acid dicarboxylic ester and preparation method thereof |
| CN103769094A (en) * | 2014-01-20 | 2014-05-07 | 中国科学院宁波材料技术与工程研究所 | Eggshell type catalyst for selective hydrogenation reaction as well as preparation method and application thereof |
| CN104399468A (en) * | 2014-11-24 | 2015-03-11 | 南京工业大学 | Nickel-based catalyst, and preparation method and application thereof |
| CN110078617A (en) * | 2019-05-14 | 2019-08-02 | 常州大学 | A method of cyclohexane cyclohexanedimethanodibasic ester is prepared with phthalic acid ester catalytic hydrogenation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112973697A (en) * | 2021-03-01 | 2021-06-18 | 广东工业大学 | Catalyst for hydrogenation reaction and synthesis method for catalyzing fatty acid methyl ester by using catalyst |
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