CN104437655A - Preparation method of magnetic solid acid catalyst for konjac flying powder - Google Patents
Preparation method of magnetic solid acid catalyst for konjac flying powder Download PDFInfo
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- CN104437655A CN104437655A CN201410654258.3A CN201410654258A CN104437655A CN 104437655 A CN104437655 A CN 104437655A CN 201410654258 A CN201410654258 A CN 201410654258A CN 104437655 A CN104437655 A CN 104437655A
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Abstract
The invention provides a preparation method of a magnetic solid acid catalyst for konjac flying powder, and belongs to the field of preparation of catalysts. In order to solve the problem that residual acid is difficult to separate by adopting the liquid acid catalyst, the catalyst cannot be repeatedly used and is high in cost because liquid hydrochloric acid is adopted for the acid of the traditional hydrolyzing konjac flying powder generally, the preparation method comprises the following steps of respectively proportioning ferric chloride, ferrous chloride and ammonia water into aqueous solutions; mixing and stirring; gradually dropwise adding oleic acid to obtain black solutions A; performing separation by using an external magnetic field to obtain a black solid A; adding the black solid A into hydrochloric acid for performing ultrasonic treatment, and separating to obtain a black solid B; drying and grinding the black solid B to obtain a magnetic solid acid catalyst of the konjac flying powder. The preparation method is easy to operate and low in cost; the prepared magnetic solid acid catalyst is high in magnetic response and has a repeated catalytic function in the acid treatment process of the konjac flying powder.
Description
Technical field
The invention belongs to the preparation field of catalyst, be specifically related to a kind of preparation method of magnetic solid acid catalyst of fry starch of konjak.
Background technology
Konjaku (Amorphopallus konjac) is herbaceos perennial, have another name called terrible taro, bennet lotus, snakehead grass, eat and cut, what be mainly utilized is its bulb part, it contains carbohydrate, protein, amino acid (17 seed amino acids, amino acid wherein containing 8 kinds of needed by human), vitamin, mineral matter etc., main component is konjaku powder (glucomannans), have control colorectal cancer and breast cancer, reduction blood-fat and blood sugar, fat-reducing effect.
The Amorphophallus Resources of China is very abundant, and be konjaku producing country maximum in the world, whole nation fine powder annual production about 5000 tons, in konjaku powder process, isolate little, the lightweight fine powder (starch, cellulose etc.) of particle be made up of parts such as konjaku epidermises and be called fry starch of konjak, its flour extraction is the 60%-80% of konjaku powder, accounts for the 30%-40% of fine powder mass fraction, and the whole nation is produced per year and flown powder 1500-2000 ton.At present konjaku powder (glucomannans) is mainly concentrated on to the utilization of konjaku, and fry starch of konjak is due to palatability extreme difference (having astringent taste, egg fishy smell and off-odor), and in food industry, utilization rate is not high, that discards in a large number flies powder not only contaminated environment, and is also great waste for Amorphophallus Resources.Along with international market is to the increase of fine powder demand, how processing fry starch of konjak (byproduct in konjaku powder processing) becomes current problem demanding prompt solution.
Fry starch of konjak is nutritious, containing a large amount of carbohydrate (mainly starch) and protein, also containing cellulose, fat, 8 kinds of essential amino acids (especially branched-chain amino acid), and the mineral matter such as calcium, magnesium, iron, zinc, phosphorus, copper, manganese, also containing multiple pharmacological active substance, as ceramide, flavone compound etc., there is effects such as improving immunity, anti-cancer, anticancer, anti-oxidant, step-down.
When exploitation fry starch of konjak, first will be hydrolyzed fry starch of konjak process.At present, the hydrolysis of fry starch of konjak mainly adopts enzyme hydrolysis, and the peptide obtained can be used for the making and research of konjaku polypeptide wine; With acid hydrolysis fly powder and fly powder Spirit brewed new research direction into.But the acid of hydrolysis fry starch of konjak is generally adopt liquid hydrochloric acid, and liquid acid catalyst exists residual acid separation difficulty, and catalyst can not be reused, the problem that catalyst cost is high.
Summary of the invention
For solving the problem, the invention provides a kind of preparation method of magnetic solid acid catalyst of fry starch of konjak, adopting following technical scheme:
A preparation method for the magnetic solid acid catalyst of fry starch of konjak, is characterized in that, comprises the following steps:
A, iron chloride, frerrous chloride and ammoniacal liquor are mixed with the aqueous solution respectively, are then uniformly mixed, obtain mixed liquor A;
B, in mixed liquor A, dropwise add oleic acid, continue stirring 3 ~ 5h, obtain dark solution A, be separated from dark solution A with externally-applied magnetic field and obtain black solid A;
C, add in hydrochloric acid by black solid A, ultrasonic process 3 ~ 10h, obtains dark solution B, is separated obtains black solid B with externally-applied magnetic field from dark solution B;
D, black solid B is dry, grind to form 50-100 object fine powder, obtain the magnetic solid acid catalyst of described fry starch of konjak.
as preferably, the mixed proportion of the aqueous solution of the iron chloride described in step a, frerrous chloride and ammoniacal liquor, by the molfraction of solute, is 2:1:8.
as preferably, the time that is uniformly mixed described in step a is 5 ~ 10h; Described be uniformly mixed while adopt oil bath heating, heating-up temperature is 30 ~ 50 DEG C.
As preferably, being separated from dark solution B with externally-applied magnetic field described in step c obtains black solid B and comprises following content: collect solid with externally-applied magnetic field from dark solution B after, with washes of absolute alcohol solid 2 ~ 3 times, then washed with de-ionized water solid is used until pH=6.7 ~ 7 of cleaning fluid, collect solid with externally-applied magnetic field, be described black solid B.
The present invention has following beneficial effect:
1. the preparation method of the magnetic solid acid catalyst of fry starch of konjak provided by the invention; oleic acid is adopted to modify tri-iron tetroxide surface; carry out coated to nano particle; make outer surface form protective layer and stop particle aggregation; the magnetic fluid particle diameter be prepared from is made to be nano level; good dispersion in the solution, increases the contact area with nucleic acid.
2. in the preparation method of the magnetic solid acid catalyst of fry starch of konjak provided by the invention, hydrochloric acid is adopted to carry out surface modification to magnetic particle, obtain the magnetic particle that there is hydrogen base on surface, in the acid treatment of fry starch of konjak, after completing catalytic treatment, externally-applied magnetic field is utilized to be separated by magnetic solid acid catalyst, the magnetic solid acid catalyst that separation obtains can also repeat catalytic reaction below, after catalytic reaction several times, after hydrogen base in catalyst comes off, catalyst can be used HCl treatment again, then can drop into equally in the acid treatment of fry starch of konjak, the cost of further reduction hydrochloric acid.
Detailed description of the invention
following examples only for illustration of the present invention, and are not used in present protection scope of the present invention.
embodiment 1
A preparation method for the magnetic solid acid catalyst of fry starch of konjak, is characterized in that, comprises the following steps:
A, iron chloride, frerrous chloride and ammoniacal liquor are mixed with the aqueous solution respectively, are then uniformly mixed under oil bath heating condition (mixed proportion of the aqueous solution of described iron chloride, frerrous chloride and ammoniacal liquor, by the molfraction of solute, is 2:1:8); Heating-up temperature is 30 DEG C, and the time of being uniformly mixed is 10h; Then be uniformly mixed, obtain mixed liquor A;
B, in mixed liquor A, dropwise add oleic acid, continue to stir 3h, obtain dark solution A, be separated from dark solution A with externally-applied magnetic field and obtain black solid A;
C, black solid A is added in hydrochloric acid, ultrasonic process 10h, obtain dark solution B, collect solid with externally-applied magnetic field from dark solution B after, with washes of absolute alcohol solid 2 ~ 3 times, then use washed with de-ionized water solid until pH=6.7 ~ 7 of cleaning fluid, collect solid with externally-applied magnetic field, be described black solid B;
D, black solid B is dry, grind to form 50 object fine powders, obtain the magnetic solid acid catalyst of described fry starch of konjak.
embodiment 2
A preparation method for the magnetic solid acid catalyst of fry starch of konjak, is characterized in that, comprises the following steps:
B, iron chloride, frerrous chloride and ammoniacal liquor are mixed with the aqueous solution respectively, are then uniformly mixed under oil bath heating condition (mixed proportion of the aqueous solution of described iron chloride, frerrous chloride and ammoniacal liquor, by the molfraction of solute, is 2:1:8); Heating-up temperature is 50 DEG C, and the time of being uniformly mixed is 5h; Then be uniformly mixed, obtain mixed liquor A;
B, in mixed liquor A, dropwise add oleic acid, continue to stir 5h, obtain dark solution A, be separated from dark solution A with externally-applied magnetic field and obtain black solid A;
C, black solid A is added in hydrochloric acid, ultrasonic process 3h, obtain dark solution B, collect solid with externally-applied magnetic field from dark solution B after, with washes of absolute alcohol solid 2 ~ 3 times, then use washed with de-ionized water solid until pH=6.7 ~ 7 of cleaning fluid, collect solid with externally-applied magnetic field, be described black solid B;
D, black solid B is dry, grind to form 100 object fine powders, obtain the magnetic solid acid catalyst of described fry starch of konjak.
embodiment 3
A preparation method for the magnetic solid acid catalyst of fry starch of konjak, is characterized in that, comprises the following steps:
C, iron chloride, frerrous chloride and ammoniacal liquor are mixed with the aqueous solution respectively, are then uniformly mixed under oil bath heating condition (mixed proportion of the aqueous solution of described iron chloride, frerrous chloride and ammoniacal liquor, by the molfraction of solute, is 2:1:8); Heating-up temperature is 40 DEG C, and the time of being uniformly mixed is 8h; Then be uniformly mixed, obtain mixed liquor A;
B, in mixed liquor A, dropwise add oleic acid, continue to stir 4h, obtain dark solution A, be separated from dark solution A with externally-applied magnetic field and obtain black solid A;
C, black solid A is added in hydrochloric acid, ultrasonic process 5h, obtain dark solution B, collect solid with externally-applied magnetic field from dark solution B after, with washes of absolute alcohol solid 2 ~ 3 times, then use washed with de-ionized water solid until pH=6.7 ~ 7 of cleaning fluid, collect solid with externally-applied magnetic field, be described black solid B;
D, black solid B is dry, grind to form 80 object fine powders, obtain the magnetic solid acid catalyst of described fry starch of konjak.
Claims (4)
1. a preparation method for the magnetic solid acid catalyst of fry starch of konjak, is characterized in that, comprises the following steps:
A, iron chloride, frerrous chloride and ammoniacal liquor are mixed with the aqueous solution respectively, are then uniformly mixed, obtain mixed liquor A;
B, in mixed liquor A, dropwise add oleic acid, continue stirring 3 ~ 5h, obtain dark solution A, be separated from dark solution A with externally-applied magnetic field and obtain black solid A;
C, add in hydrochloric acid by black solid A, ultrasonic process 3 ~ 10h, obtains dark solution B, is separated obtains black solid B with externally-applied magnetic field from dark solution B;
D, black solid B is dry, grind to form 50-100 object fine powder, obtain the magnetic solid acid catalyst of described fry starch of konjak.
2. the preparation method of the magnetic solid acid catalyst of fry starch of konjak according to claim 1, is characterized in that, the mixed proportion of the aqueous solution of the iron chloride described in step a, frerrous chloride and ammoniacal liquor, by the molfraction of solute, is 2:1:8.
3. the preparation method of the magnetic solid acid catalyst of fry starch of konjak according to claim 1, is characterized in that, the time that is uniformly mixed described in step a is 5 ~ 10h; Described be uniformly mixed while adopt oil bath heating, heating-up temperature is 30 ~ 50 DEG C.
4. the preparation method of the magnetic solid acid catalyst of fry starch of konjak according to claim 1, it is characterized in that, being separated from dark solution B with externally-applied magnetic field described in step c obtains black solid B and comprises following content: collect solid with externally-applied magnetic field from dark solution B after, with washes of absolute alcohol solid 2 ~ 3 times, then washed with de-ionized water solid is used until pH=6.7 ~ 7 of cleaning fluid, collect solid with externally-applied magnetic field, be described black solid B.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1290574A (en) * | 2000-11-08 | 2001-04-11 | 哈尔滨工程大学 | Magnetic solid super strong acid catalyst and its preparing method |
| CN1613559A (en) * | 2004-09-28 | 2005-05-11 | 北京化工大学 | Preparation for hydrophobic solid acid catalyst |
| CN102553647A (en) * | 2012-01-09 | 2012-07-11 | 华东师范大学 | Magnetic nanometer solid acid catalyst and preparation method thereof |
| CN103865916A (en) * | 2014-03-24 | 2014-06-18 | 吉林大学 | Magnetic drive immobilized enzyme, preparation method and application of magnetic drive immobilized enzyme to large-water body catalysis |
-
2014
- 2014-11-18 CN CN201410654258.3A patent/CN104437655A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1290574A (en) * | 2000-11-08 | 2001-04-11 | 哈尔滨工程大学 | Magnetic solid super strong acid catalyst and its preparing method |
| CN1613559A (en) * | 2004-09-28 | 2005-05-11 | 北京化工大学 | Preparation for hydrophobic solid acid catalyst |
| CN102553647A (en) * | 2012-01-09 | 2012-07-11 | 华东师范大学 | Magnetic nanometer solid acid catalyst and preparation method thereof |
| CN103865916A (en) * | 2014-03-24 | 2014-06-18 | 吉林大学 | Magnetic drive immobilized enzyme, preparation method and application of magnetic drive immobilized enzyme to large-water body catalysis |
Non-Patent Citations (2)
| Title |
|---|
| SUDIPTA PATHAK ET AL: "Facile cyclization in the synthesis of highly fused diaza cyclooctanoid compounds using retrievable nano magnetite- supported sulfonic acid catalyst", 《RSC ADV.》 * |
| 毛丹等: "双层表面活性剂改性Fe3O4磁流体的制备", 《科技创新导报》 * |
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