CN101327422A - Method for preparing rapid filtration concave earth adsorbing agent for decolouration of tallow oil - Google Patents
Method for preparing rapid filtration concave earth adsorbing agent for decolouration of tallow oil Download PDFInfo
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- CN101327422A CN101327422A CNA2008100212550A CN200810021255A CN101327422A CN 101327422 A CN101327422 A CN 101327422A CN A2008100212550 A CNA2008100212550 A CN A2008100212550A CN 200810021255 A CN200810021255 A CN 200810021255A CN 101327422 A CN101327422 A CN 101327422A
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- attapulgite
- filter cake
- filter mass
- tallow oil
- recessed soil
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Abstract
The present invention discloses a preparation method of a fast filtering attapulgite absorbent used for decolorizing. The preparation method comprises the steps as follows: firstly, in acidification treatment, every 1g of attapulgite is processed by 5ml of sulfuric acid solution of 3 percent to 7 percent of concentration and is stirred in 300rpm under the acidification temperature of 90 DEG C for 3 to 4 hours, the attapulgite is filtered after being acidified, and a filter mass is washed by tap water until pH is neutral; then, in filter mass chemical treatment, the filter mass is added into the tap water, 5 to 15g of lemery is added into every 200g of the attapulgite to be stirred and react for 2 hours and to be filtered after the reaction; finally, in filter mass heat treatment, the filter mass is dried for 2 hours under the constant temperature of 105 DEG C, the dried filter mass is calcined and activated in a muffle under 280 DEG C to 320 DEG C for 1 hour to be grinded and filtered to 100 meshes for obtaining the fast filtering attapulgite absorbent. The present invention improves the decolorizing effect of the fast filtering attapulgite absorbent by the acidification and the heat treatment and the chemical treatment on the attapulgite to ensure that the fast filtering attapulgite absorbent replaces floridin to reduce the industrial production cost.
Description
Technical field
The present invention relates to the preparation of adsorbent method, be specifically related to the preparation method of a kind of tallow oil decolouring with fast filter property attapulgite adsorbent.
Background technology
Foam is abundant in order to prepare, the soap series products of strong detergency, needs various greases to arrange in pairs or groups mutually, and representative formula is 80% tallow oil and 20% coconut oil.Along with growth in the living standard, people also improve greatly to the quality requirement of perfumed soap, and the requirement to grease colourity in the production is also more and more stricter.
Now, the tallow oil major part of domestic use is from Australia and New Zealand, also has from the U.S. and Canadian import.The pigment of sneaking in the tallow oil comprises non-natural pigment two classes that produce in natural colouring matter and the storage process.The discoloration method of grease is mainly absorption method and chemical method, and saponification is industrial, and what be most widely used is absorption method, and the key of this method is to select suitable adsorbent and suitable process condition.
Industrial saponification is mainly atlapulgite with the grease-decolor adsorbent, consumption requires to decide with grease kind, quality and decolouring, is generally 3%～5%, reaches as high as 10%, atlapulgite is to the tallow oil good decolorizing effect, but price is about 3 times of attapulgite clay (being called for short recessed soil).
Recessed soil be a kind of layer of chain structure contain Shuifu County's zeopan clay mineral, have special fibre structure, unusual colloid and absorption property.Recessed soil in Chinese Jiangsu, Anhui and Fla. reserves are very big.Wherein output ranks first with Xuyi Jiangsu, accounts for 70% of the recessed native reserves of China, accounts for the nearly 50% of the recessed native gross reserves in the whole world, is world's high-quality mineral reserve.
The adsorbent of recessed soil preparation has been widely used in the aspects such as decolorizing purification of vegetable oil decolorization refining and gasoline, diesel oil, aviation kerosine, but it is very few to be used for tallow oil Study on Decolorization report.The viscosity of tallow oil and vegetable oil, molecular weight size all have significant difference, and main pigment molecular size is also different, recessed soil is better to the vegetable oil decolorizing effect, but effect is not good enough aspect the tallow oil decolouring, recessed soil is because the colloidal property stickiness height of itself, when filter the back of having decoloured, cause the rate of filtration slow partially, influence production efficiency.
Summary of the invention
The objective of the invention is to: the preparation method of a kind of tallow oil decolouring with fast filter property attapulgite adsorbent is provided,, improves its percent of decolourization, improve its strainability simultaneously tallow oil by the hole structural property of this method modified attapulgite.
The principle of technical solution of the present invention is: by sulfuric acid and heat treatment phase combination, change the pore-size distribution of recessed soil, make its decolouring that is suitable for tallow oil, introduce chemical treatment simultaneously, reduce the generation of the surperficial colloid of decolorization concave soil, improve the decolouring back rate of filtration.
Preparation method of the present invention comprises following concrete steps: at first, the recessed soil of acidification, the recessed soil of every 1g is handled with the sulfuric acid solution of 5ml concentration 3-7%, 300rpm stirs, 90 ℃ of souring temperatures, time 3-4h, acidifying finishes the back and filters, filter cake washes the neutrality to pH with running water, then, and the filter cake chemical treatment, filter cake is added running water, the recessed soil of every 200g adds the potassium sulfate of 5-15g, stirring reaction 2h, and reaction finishes the back and filters; At last, filter cake heat treatment, filter cake is in 105 ℃ of freeze-day with constant temperature 2h, and dried filter cake is 280-320 ℃ of calcination activation 1h in Muffle furnace, and grinding is screened to 100 orders and gets filter property attapulgite adsorbent soon.
The recessed native raw ore powder before the activation is not tightly to reunite together, is the soil block shape, and the surface is smooth relatively, is unfavorable for the tallow oil adsorption bleaching, shown in the ESEM that Fig. 1 amplifies 5,000 times.
Acid, heat treatment can both change the pore structure of recessed soil, thereby improve its absorption property.When the main duct of recessed soil greater than pigment molecular, just can make pigment molecular fully enter recessed native duct is removed, but decolour for tallow oil, the duct that is not sorbing material is the bigger the better, have only duct and pigment molecular approaching more, the pigment molecular that enters in the duct just is not easy desorption, and percent of decolourization just can improve.Handle through appropriate sulfuric acid, thermal activation modification, the brilliant bundle in recessed soil surface spreads out, obviously roughening, the surface generates many ducts simultaneously, shown in the sem photograph that Fig. 2 amplifies 5,000 times, this is because acid activation can be removed the impurity such as carbonate in the former recessed soil, plays the effect of mediation duct and increase specific surface, helps the tallow oil adsorption bleaching.
Octahedral layer edge cation in the recessed soil structure (is mainly Mg
2+) along with sulfuric acid concentration increases and constantly reduces, the octahedral rate of dissolution of Al is less than the octahedra rate of dissolution of Mg, sulfuric acid and recessed native course of reaction belong to proton outer surface penetration mechanism from the inwardly diffusion of crystal external margin, too high sulfuric acid concentration activation, can make octahedral cations be bordering on dissolving fully, Mg, Al relative amount sharply descend, and tetrahedron loses support, and crystal structure may collapse, endoporus disappears, and its decoloring ability to tallow oil is obviously reduced.
Attapulgite after the high-temperature roasting, porosity and equivalent pore diameter can obviously improve.Recessed soil is moisture rich zeopan, and three kinds of water exist in the recessed native different structure in the molecular formula: duct water can be deviate under 50 ℃～180 ℃; Crystallization water when cavity walls and cation coordination is deviate under 210 ℃～350 ℃; Constitution water is deviate under 350 ℃～550 ℃.The water of three kinds of different conditions, in crystal structure, duct water, the crystallization water are easily deviate from, and improve with the raising effusion water yield of sintering temperature, constitution water will could be overflowed at the high temperature more than 350 ℃, whole dehydrations about 600 ℃, crystal structure destroys in the time of 700 ℃, generates cenotype.Sintering temperature and decolorizing ability have correlation preferably, and its decolorizing ability improves with sintering temperature, reach the top in the time of general 400 ℃, and temperature raises again, the hurried decline of decolorizing ability meeting, and adsorption effect also descends.
In the sulfuric acid priming reaction process, H+ has replaced the Al in the recessed native octahedron
3+, generate aluminum sulfate, in decolorization, form steady suspension, the decentralized photo of this suspension is made of the particle and the lip-deep aluminum sulfate thereof of recessed soil, and during the recessed soil after the sulfuric acid activation used, this colloidal property can make the rate of filtration obviously slack-off.In recessed native activation process, add potassium sulfate following reaction arranged:
3Al
2(SO
4)
3+ K
2SO
4+ 7H
2O=K
2Al (SO
4)
4(OH)
2+ 6H
2SO
4Can form the insoluble basic aluminium sulphate inorganic compound of electric double layer potassium on recessed soil particle surface like this, thereby improve the strainability of sulfuric acid activation recurve soil in the tallow oil decolouring is used.
The present invention has the following advantages: 1. handle by recessed soil being carried out suitable acid and thermal activation modification, can improve its decolorizing effect to tallow oil, thereby make it can substitute atlapulgite, reduce production costs; 2. the present invention introduces appropriate chemical treatment, can obviously improve the strainability of recessed soil, improves decolouring production efficiency.
Description of drawings
Fig. 1 amplifies 5,000 times sem photograph for recessed native raw ore powder.
Fig. 2 amplifies 5,000 times sem photograph for attapulgite adsorbent.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that these embodiment just in order to demonstrate the invention, but not limit the scope of the invention by any way.
Embodiment 1:
The preparation sulfuric acid concentration is 5% solution 1L, takes by weighing the recessed soil of 200g and joins in the sulfuric acid solution that configures and do not stop to stir with 300rpm, and souring temperature is 90 ℃, time 4h, and acidifying finishes the back filters, and filter cake washes the neutrality to pH with running water; Filter cake is added the 100ml running water, add the 10g potassium sulfate again, continue stirring reaction 2h, reaction finishes the back and filters; 105 ℃ of freeze-day with constant temperature 2h of filter cake, oven dry filter cake 300 ℃ of roasting 1h in Muffle furnace grind and are screened to 100 orders to put into vacuum desiccator stand-by.
With the BELSORP-II specific surface of Dutch ANKERSMID company and the recessed soil after the pore-size distribution instrument test modification, its specific area is 215.36m
2/ g, average pore diameter are 9.45nm.
Take by weighing above-mentioned 15g modified attapulgite and put into round-bottomed flask with the 500ml tallow oil, the control bleaching temperature is 100 ℃, does not stop to stir 30min with 300rpm, after decolouring finishes, and vacuum filtration, testing its percent of decolourization is 96%, filtration time is 4.6min.
Embodiment 2:
Change the sulfuric acid concentration of activation usefulness into 10%, all the other conditions are constant with embodiment 1, after decolouring finishes, and vacuum filtration, testing its percent of decolourization is 89%, and filtration time is 4.4min, and the specific area of recessed soil is 232.52m
2/ g, average pore diameter are 12.45nm.Through relatively learning, the acid concentration of activation usefulness is higher, and recessed native specific surface and aperture all increase, but decolorizing effect slightly descends.
Embodiment 3:
Change the sulfuric acid concentration of activation usefulness into 20%, all the other conditions are constant with embodiment 1, after decolouring finishes, and vacuum filtration, testing its percent of decolourization is 78%, and filtration time is 4.1min, and the specific area of recessed soil is 221.78m
2/ g, average pore diameter are 14.31nm.Through relatively learning, when the acid concentration of activation usefulness was too high, recessed native crystal structure may be destroyed, and its specific surface decreases, but average pore size still increases, and decolorizing effect but obviously reduces, and there is bigger relation in visible percent of decolourization and aperture, are not to be the bigger the better.
Embodiment 4:
Take by weighing the recessed soil of 200g and activate, but add in the 100ml aqueous solution, add the 10g potassium sulfate again without sulfuric acid, do not stop to stir 2h with 300rpm, filter, in 105 ℃ of freeze-day with constant temperature 2h, 300 ℃ of calcination activation 1h in Muffle furnace grind and to be screened to that to put into vacuum desiccator behind 100 orders stand-by.Take by weighing the recessed soil of 15g and put into round-bottomed flask with the 500ml tallow oil, the control bleaching temperature is 100 ℃, does not stop to stir 30min with 300rpm, after decolouring finishes, vacuum filtration, testing its percent of decolourization is 48%, filtration time is 5.6min, and the specific area of recessed soil is 162.68m
2/ g, average pore diameter are 7.21nm.As seen without acid activation, only the recessed soil of thermal activation is relatively poor to the percent of decolourization of tallow oil, and strainability is also bad.
Embodiment 5:
Except after the acid activation in Muffle furnace sintering temperature be 400 ℃, all the other conditions are constant with embodiment 1, after decolouring finishes, vacuum filtration, testing its percent of decolourization is 88%, filtration time is 4.3min.As seen after the sulfuric acid activation, during thermal activation, temperature is unsuitable too high again, otherwise percent of decolourization decreases on the contrary.
Embodiment 6:
Except not adding potassium sulfate, all the other conditions are constant with embodiment 1, after decolouring finishes, and vacuum filtration, testing its percent of decolourization is 94%, filtration time is 7.5min.Whether little to the percent of decolourization influence of tallow oil the adding of potassium sulfate is, but to the filtering rate influence obviously, do not add potassium sulfate, and filtration time has almost prolonged 1 times.
Embodiment 7:
Except the addition of potassium sulfate is 5g, all the other conditions are constant with embodiment 1, after decolouring finishes, and vacuum filtration, testing its percent of decolourization is 95%, filtration time is 6.2min.
Embodiment 8:
Except the addition of potassium sulfate is 15g, all the other conditions are constant with embodiment 1, after decolouring finishes, and vacuum filtration, testing its percent of decolourization is 93%, filtration time is 3.9min.
Claims (1)
1. the tallow oil decolouring is characterized in that: by sulfuric acid and heat treatment phase combination, change the pore-size distribution of recessed soil, introduce chemical treatment simultaneously, reduce the generation of the surperficial colloid of decolorization concave soil with the preparation method of fast filter property attapulgite adsorbent; Comprise following concrete steps: at first, acidification, the recessed soil of every 1g is handled with the sulfuric acid solution of 5ml concentration 3-7%, and 300rpm stirs, 90 ℃ of souring temperatures, time 3-4h, acidifying finishes the back filters, and filter cake washes the neutrality to pH with running water; Then, the filter cake chemical treatment adds running water with filter cake, and the recessed soil of every 200g adds the potassium sulfate of 5-15g, stirring reaction 2h, and reaction finishes the back and filters; At last, filter cake heat treatment, filter cake is in 105 ℃ of freeze-day with constant temperature 2h, and dried filter cake is 280-320 ℃ of calcination activation 1h in Muffle furnace, and grinding is screened to 100 and gets filter property attapulgite adsorbent soon.
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| CNB2008100212550A CN100563816C (en) | 2008-07-23 | 2008-07-23 | The tallow oil decolouring preparation method of fast filter property attapulgite adsorbent |
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| CN100563816C CN100563816C (en) | 2009-12-02 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225327A (en) * | 2011-04-21 | 2011-10-26 | 郑玥 | Method for producing attapulgite palm oil de-coloring purifying agent |
| CN101502787B (en) * | 2009-02-09 | 2012-07-04 | 朱永林 | Method for preparing high-intensity water-resistant multifunctional high-efficient granule active clay preparation and use thereof |
| CN102806063A (en) * | 2012-09-04 | 2012-12-05 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Preparation method of attapulgite clay adsorbent for degumming and decoloration of palm oil |
| CN103894142A (en) * | 2014-03-06 | 2014-07-02 | 中山职业技术学院 | Organically modified attapulgite clay soy sauce residue oil decolorant and preparation method thereof |
| CN105148830A (en) * | 2015-06-18 | 2015-12-16 | 深圳清华大学研究院 | Decoloring clay adsorbent and preparation method thereof |
-
2008
- 2008-07-23 CN CNB2008100212550A patent/CN100563816C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502787B (en) * | 2009-02-09 | 2012-07-04 | 朱永林 | Method for preparing high-intensity water-resistant multifunctional high-efficient granule active clay preparation and use thereof |
| CN102225327A (en) * | 2011-04-21 | 2011-10-26 | 郑玥 | Method for producing attapulgite palm oil de-coloring purifying agent |
| CN102225327B (en) * | 2011-04-21 | 2012-10-17 | 郑玥 | Method for producing attapulgite palm oil de-coloring purifying agent |
| CN102806063A (en) * | 2012-09-04 | 2012-12-05 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Preparation method of attapulgite clay adsorbent for degumming and decoloration of palm oil |
| CN103894142A (en) * | 2014-03-06 | 2014-07-02 | 中山职业技术学院 | Organically modified attapulgite clay soy sauce residue oil decolorant and preparation method thereof |
| CN103894142B (en) * | 2014-03-06 | 2016-06-15 | 中山职业技术学院 | A kind of organically-modified attapulgite clay soy sauce residues fat decolourizing agent and preparation method thereof |
| CN105148830A (en) * | 2015-06-18 | 2015-12-16 | 深圳清华大学研究院 | Decoloring clay adsorbent and preparation method thereof |
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| CN100563816C (en) | 2009-12-02 |
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