CN104475127A - Method for preparing solid acid catalyst - Google Patents
Method for preparing solid acid catalyst Download PDFInfo
- Publication number
- CN104475127A CN104475127A CN201410656261.9A CN201410656261A CN104475127A CN 104475127 A CN104475127 A CN 104475127A CN 201410656261 A CN201410656261 A CN 201410656261A CN 104475127 A CN104475127 A CN 104475127A
- Authority
- CN
- China
- Prior art keywords
- pineapple bran
- acid catalyst
- solid acid
- sulfuric acid
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Catalysts (AREA)
Abstract
The invention relates to a method for preparing a solid acid catalyst. The method comprises the steps of preparing active carbon by using pineapple residues and preparing the solid acid catalyst by using the prepared active carbon. The solid acid catalyst prepared according to the method can replace the conventional liquid acid catalyst to be used in the esterification reaction of fatty acid and short-chain alcohol and no acidy waste water is produced; and the solid acid catalyst can be recycled, and can be reused through acid regeneration after being used for a plurality of times.
Description
Technical field
The invention belongs to a kind of preparation method of catalyst, be specifically related to a kind of preparation method of solid acid catalyst.
Background technology
Biodiesel is the one of biomass energy, compared with petrifaction diesel, with its not sulfur-bearing and aromatic hydrocarbons, Cetane number high, biodegradable, to the advantage such as environmental hazard is little, reach the health effect testing requirement of the U.S.'s " clean air act " defined, and its flash-point is high, store, use, transport all very safe, so become one of most popular substitute energy source for petroleum.
Traditional biological diesel production technique adopts liquid soda acid as catalyst, mainly there is following problem: the liquid acid that a. adds in a large number easily produces coking; B., after having reacted, need to add a large amount of alkali neutralisation of sulphuric acid; C. the residue after decompression distillation has the impure difficulty of a lot of carbonizing matter, glycerine to recycle; D. the waste water of a large amount of acidity or high salt concentration can be produced; E. catalyst can not reuse, and cost is higher.For addressing these problems, current employing is more replace homogeneous acid with solid acid.Solid acid alkali catalytic agent is the basis of green bio diesel oil process route.
In pineapple process, a large amount of pineapple brans just constantly produces, and accounts for the ratio of fresh fruit 60%.A large amount of pineapple bran goes out of use, and is well utilized.
Summary of the invention
For solving the problem, the invention provides a kind of preparation method discarded pineapple bran being used for solid acid catalyst, pineapple bran being turned waste into wealth, makes full use of resource, improve the byproduct income of orchard worker.The present invention adopts following technical scheme:
A preparation method for solid acid catalyst, is characterized in that comprising the following steps:
(1) by pineapple bran dry to water content lower than 15%, be then crushed to 80 ~ 100 orders;
(2) mixed liquor of drying the pineapple bran phosphoric acid after pulverizing and sulfuric acid is stirred, dipping 10 ~ 12h;
(3) pineapple bran flooded is carried out charing 45 ~ 60min at 300 DEG C, be then warming up to 450 ~ 500 DEG C and carry out activation 10 ~ 15min;
(4) pineapple bran after activation being washed with distilled water to pH value is 6 ~ 7, then dries and obtain pineapple bran activation charcoal;
(5) pineapple bran is activated charcoal at 150 ~ 200 DEG C, through sulfonating agent solution sulfonation 5 ~ 10h;
(6) washing to pH value with the distilled water of 70 ~ 80 DEG C after sulfonation is 6 ~ 7, and then oven dry is crushed to 200 orders and namely obtains described solid acid catalyst.
Further, the mixed liquor of phosphoric acid and sulfuric acid is volumn concentration in described step (2) be the phosphoric acid of 35% and the sulfuric acid of 98% is that 8:1 mixes according to volume ratio; Described pineapple bran is 1:(1.5 ~ 2 with the mixed volume ratio of mixed liquor).
Further, in described step (5), sulfonating agent is the concentrated sulfuric acid.
Beneficial effect of the present invention is as follows:
1. the pineapple bran in the present invention is convenient to collect, and reduces costs, is turned waste into wealth by pineapple bran, make full use of resource, improves the byproduct income of orchard worker.
2. adopt phosphoric acid and sulfuric acid mixture liquid to flood in the present invention, simple to operation, the pineapple bran active carbon obtained has abundant gap structure and larger specific area, and active carbon productive rate reaches 50 ~ 55%.
3. the present invention's pineapple bran makes active carbon, then prepares solid acid catalyst with obtained active carbon, and the esterification of alternative traditional liquid acid catalyst catalyze fatty acid and short chain alcohol, can not produce acid waste water; And this solid acid catalyst can repeated collection use, and again can also be utilized after repeatedly using by acid regeneration.
Detailed description of the invention
Following examples are to particular content of the present invention is described better, be not limited to protection scope of the present invention.
embodiment 1
A preparation method for solid acid catalyst, comprises the following steps:
(1) by pineapple bran dry to water content lower than 15%, be then crushed to 80 orders;
(2) mixed liquor of drying the pineapple bran phosphoric acid after pulverizing and sulfuric acid is stirred, dipping 12h;
The mixed liquor of phosphoric acid and sulfuric acid is volumn concentration be the phosphoric acid of 35% and the sulfuric acid of 98% is that 8:1 mixes according to volume ratio; Described pineapple bran is 1:1.5 with the mixed volume ratio of mixed liquor;
(3) pineapple bran flooded is carried out charing 45min at 300 DEG C, be then warming up to 500 DEG C and carry out activation 10min;
(4) pineapple bran after activation being washed with distilled water to pH value is 6 ~ 7, then dries and obtain pineapple bran activation charcoal;
(5) pineapple bran is activated charcoal at 150 DEG C, through sulfonating agent solution sulfonation 10h;
(6) washing to pH value with the distilled water of 70 ~ 80 DEG C after sulfonation is 6 ~ 7, and then oven dry is crushed to 200 orders and namely obtains described solid acid catalyst.
embodiment 2
A preparation method for solid acid catalyst, comprises the following steps:
(1) by pineapple bran dry to water content lower than 15%, be then crushed to 100 orders;
(2) mixed liquor of drying the pineapple bran phosphoric acid after pulverizing and sulfuric acid is stirred, dipping 10h;
The mixed liquor of phosphoric acid and sulfuric acid is volumn concentration be the phosphoric acid of 35% and the sulfuric acid of 98% is that 8:1 mixes according to volume ratio; Described pineapple bran is 1:2 with the mixed volume ratio of mixed liquor;
(3) pineapple bran flooded is carried out charing 60min at 300 DEG C, be then warming up to 450 DEG C and carry out activation 10min;
(4) pineapple bran after activation being washed with distilled water to pH value is 6 ~ 7, then dries and obtain pineapple bran activation charcoal;
(5) pineapple bran is activated charcoal at 150 ~ 200 DEG C, through concentrated acid sulfonation 5 ~ 10h;
(6) washing to pH value with the distilled water of 70 ~ 80 DEG C after sulfonation is 6 ~ 7, and then oven dry is crushed to 200 orders and namely obtains described solid acid catalyst.
embodiment 3
A preparation method for solid acid catalyst, comprises the following steps:
(1) by pineapple bran dry to water content lower than 15%, be then crushed to 100 orders;
(2) mixed liquor of drying the pineapple bran phosphoric acid after pulverizing and sulfuric acid is stirred, dipping 11h;
The mixed liquor of phosphoric acid and sulfuric acid is volumn concentration be the phosphoric acid of 35% and the sulfuric acid of 98% is that 8:1 mixes according to volume ratio; Described pineapple bran is 1:1.8 with the mixed volume ratio of mixed liquor;
(3) pineapple bran flooded is carried out charing 50min at 300 DEG C, be then warming up to 480 DEG C and carry out activation 12min;
(4) pineapple bran after activation being washed with distilled water to pH value is 6 ~ 7, then dries and obtain pineapple bran activation charcoal;
(5) pineapple bran is activated charcoal at 150 ~ 200 DEG C, through sulfonating agent solution sulfonation 8h; The concentrated sulfuric acid.
(6) washing to pH value with the distilled water of 70 ~ 80 DEG C after sulfonation is 6 ~ 7, and then oven dry is crushed to 200 orders and namely obtains described solid acid catalyst.
Claims (3)
1. a preparation method for solid acid catalyst, is characterized in that comprising the following steps:
By pineapple bran dry to water content lower than 15%, be then crushed to 80 ~ 100 orders;
The mixed liquor of drying the pineapple bran phosphoric acid after pulverizing and sulfuric acid is stirred, dipping 10 ~ 12h;
The pineapple bran flooded is carried out charing 45 ~ 60min at 300 DEG C, is then warming up to 450 ~ 500 DEG C and carries out activation 10 ~ 15min;
It is 6 ~ 7 that pineapple bran after activation is washed with distilled water to pH value, then dries and obtain pineapple bran activation charcoal;
Pineapple bran is activated charcoal at 150 ~ 200 DEG C, through sulfonating agent solution sulfonation 5 ~ 10h;
Washing to pH value with the distilled water of 70 ~ 80 DEG C after sulfonation is 6 ~ 7, and then oven dry is crushed to 200 orders and namely obtains described solid acid catalyst.
2. the preparation method of solid acid catalyst according to claim 1, the mixed liquor that it is characterized in that phosphoric acid and sulfuric acid in described step (2) is volumn concentration be the phosphoric acid of 35% and the sulfuric acid of 98% is that 8:1 mixes according to volume ratio; Described pineapple bran is 1:(1.5 ~ 2 with the mixed volume ratio of mixed liquor).
3. the preparation method of solid acid catalyst according to claim 1, is characterized in that in described step (5), sulfonating agent is the concentrated sulfuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410656261.9A CN104475127A (en) | 2014-11-18 | 2014-11-18 | Method for preparing solid acid catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410656261.9A CN104475127A (en) | 2014-11-18 | 2014-11-18 | Method for preparing solid acid catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104475127A true CN104475127A (en) | 2015-04-01 |
Family
ID=52749808
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410656261.9A Pending CN104475127A (en) | 2014-11-18 | 2014-11-18 | Method for preparing solid acid catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104475127A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104941663A (en) * | 2015-04-09 | 2015-09-30 | 广东工业大学 | Preparation method of high acid content solid acid catalyst |
| CN105536822A (en) * | 2016-01-21 | 2016-05-04 | 定陶县地元生化制品有限公司 | Preparation method for solid acid catalyst for biodiesel |
| CN105618025A (en) * | 2016-01-14 | 2016-06-01 | 北京道顺国际技术开发有限责任公司 | Method for preparing biomass charcoal by catalyzing organic waste at low temperature with sulfonated char |
| CN106380394A (en) * | 2016-08-26 | 2017-02-08 | 南京工业大学 | Preparation method of carbon-silicon solid acid catalyst and application in extraction of organic acid in fermentation broth |
| CN110092379A (en) * | 2019-04-12 | 2019-08-06 | 蚌埠学院 | It is a kind of using biomass as the method and application of raw material one-step synthesis sulfonation active carbon |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH049352A (en) * | 1990-02-08 | 1992-01-14 | Kawasaki Steel Corp | Production of naphthalenedicarboxylic acid |
| CN102092712A (en) * | 2011-01-31 | 2011-06-15 | 中国林业科学研究院林产化学工业研究所 | Method for directionally preparing high specific surface area wood-pellets activated carbon at low temperature |
| CN103084187A (en) * | 2012-12-17 | 2013-05-08 | 常州大学 | Carbon-based solid acid and preparation method thereof |
| CN103756787A (en) * | 2013-12-26 | 2014-04-30 | 中国林业科学研究院林产化学工业研究所 | Method for extracting essential oil from wood processing waste Chinese fir chips to co-produce chemical method activated carbon |
-
2014
- 2014-11-18 CN CN201410656261.9A patent/CN104475127A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH049352A (en) * | 1990-02-08 | 1992-01-14 | Kawasaki Steel Corp | Production of naphthalenedicarboxylic acid |
| CN102092712A (en) * | 2011-01-31 | 2011-06-15 | 中国林业科学研究院林产化学工业研究所 | Method for directionally preparing high specific surface area wood-pellets activated carbon at low temperature |
| CN103084187A (en) * | 2012-12-17 | 2013-05-08 | 常州大学 | Carbon-based solid acid and preparation method thereof |
| CN103756787A (en) * | 2013-12-26 | 2014-04-30 | 中国林业科学研究院林产化学工业研究所 | Method for extracting essential oil from wood processing waste Chinese fir chips to co-produce chemical method activated carbon |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104941663A (en) * | 2015-04-09 | 2015-09-30 | 广东工业大学 | Preparation method of high acid content solid acid catalyst |
| CN105618025A (en) * | 2016-01-14 | 2016-06-01 | 北京道顺国际技术开发有限责任公司 | Method for preparing biomass charcoal by catalyzing organic waste at low temperature with sulfonated char |
| CN105618025B (en) * | 2016-01-14 | 2018-04-17 | 北京道顺国际技术开发有限责任公司 | A kind of method that low-temperature catalyzed organic waste of sulfonation charcoal prepares biomass carbon |
| CN105536822A (en) * | 2016-01-21 | 2016-05-04 | 定陶县地元生化制品有限公司 | Preparation method for solid acid catalyst for biodiesel |
| CN105536822B (en) * | 2016-01-21 | 2017-09-29 | 定陶县地元生化制品有限公司 | A kind of preparation method of solid acid catalyst for biodiesel |
| CN106380394A (en) * | 2016-08-26 | 2017-02-08 | 南京工业大学 | Preparation method of carbon-silicon solid acid catalyst and application in extraction of organic acid in fermentation broth |
| CN106380394B (en) * | 2016-08-26 | 2018-11-06 | 南京工业大学 | A kind of preparation method of carbon-silicon solid acid catalyst and its in extracting zymotic fluid organic acid application |
| CN110092379A (en) * | 2019-04-12 | 2019-08-06 | 蚌埠学院 | It is a kind of using biomass as the method and application of raw material one-step synthesis sulfonation active carbon |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Esmaeili | A critical review on the economic aspects and life cycle assessment of biodiesel production using heterogeneous nanocatalysts | |
| CN104475127A (en) | Method for preparing solid acid catalyst | |
| CN105461758B (en) | A method of improving lignite humic acid extract content | |
| CN101890364B (en) | Method of using agricultural and forestry waste to prepare solid-acid catalyst | |
| CN104232124B (en) | A kind of biomass cracking carbonizing and gasifying device | |
| CN102786986A (en) | Refining technology of microalgae pyrolysis oil | |
| CN104357071A (en) | Method for directionally producing biomass charcoal, biomass oil and biomass gas through microwave catalytic pyrolysis of biomass | |
| CN102190298A (en) | Method for preparing active carbon from carbon byproduct in fast pyrolysis of forest remainder | |
| CN103626633A (en) | Method for promoting solid catalyst to depolymerize cellulose | |
| Yadav et al. | Fabrication of surface-modified dual waste-derived biochar for biodiesel production by microwave-assisted esterification of oleic acid: Optimization, kinetics, and mechanistic studies | |
| CN101812320B (en) | Waste oil regenerated energy device and processing method | |
| CN102358619A (en) | Method for preparing hydrophobic active carbon by using avian hairs | |
| CN103205275A (en) | Method for preparing phenol compound and clean fuel oil from coal tar | |
| CN102321489B (en) | Method for catalyzing and liquefying agricultural wastes by using ion liquid | |
| CN102533442A (en) | Method for purifying biodiesel | |
| CN103980929A (en) | Method for preparing biological fuel oil by fast pyrolyzing biomass | |
| CN204198666U (en) | A kind of biomass cracking carbonizing and gasifying device | |
| CN109535439A (en) | A kind of extracting method of humic acid | |
| CN101665716B (en) | Composite deacidification agent and method for recovering naphthenic acid from oil | |
| CN101787301B (en) | Processing method of lignite | |
| CN103937525B (en) | A kind of method adopting acidic ion liquid depolymerization brown coal | |
| CN102268329B (en) | Method for preparing biodiesel | |
| CN202610209U (en) | High acid value oil and fat preparation biodiesel device | |
| CN101508904A (en) | Method for producing biodiesel | |
| CN105273838A (en) | Biodiesel adsorption deacidification method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150401 |