CN105016352B - A kind of food-grade montmorillonite and its preparation process - Google Patents
A kind of food-grade montmorillonite and its preparation process Download PDFInfo
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- CN105016352B CN105016352B CN201510496004.8A CN201510496004A CN105016352B CN 105016352 B CN105016352 B CN 105016352B CN 201510496004 A CN201510496004 A CN 201510496004A CN 105016352 B CN105016352 B CN 105016352B
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Abstract
The present invention relates to a kind of montmorillonites, and specifically a kind of food-grade montmorillonite, purity are more than 99.0%, heavy metal lead and are less than 5ppn, whiteness more than 80%, cation exchange capacity more than 120mmol/100g.Its preparation process, includes the following steps：（1）After drying montmorillonite raw material under the conditions of 70 90 DEG C, 300 500 mesh are crushed to, obtain raw material powder；（2）Water is added in into raw material powder, is stirred and evenly mixed with raw material powder, the slurries that solid content is 10 25% are made；（3）The slurries cross 400 500 mesh sieves, obtain the first filtrate；（4）First filtrate be sent into ultra-fine equipment carry out it is ultra-fine delaminate, remove solid particle using classifying equipoment after delaminating, obtain the second filtrate；（5）By second filtrate sterilizing, concentration, drying, obtain food-grade montmorillonite product, pass through crushing, slurrying, coarse filtration, fine filtering, sterilizing series of steps, the montmorillonite product for reaching food-grade requirement in parameters such as color and luster, purity, adsorption capacities is made, product quality is stablized, entire technical process is at low cost, can mass produce.
Description
Technical field
The present invention relates to a kind of montmorillonites, and specifically a kind of food-grade montmorillonite and its preparation process, it is pure to belong to substance
Change manufacture field.
Background technology
Montmorillonite is bentonitic main component, since it is with special water imbibition, hydroplasticity, caking property and relatively strong
Ion exchange under, it is wider in current application range, be widely used in each field such as machinery, chemical industry, health care.But natural cover takes off
It is associated with the non-clay silicate mineral such as silica, opal, feldspar, gypsum, calcite in stone, purity difference, montmorillonite
Content is usually in 50%-70%, and part rich ore content is up to 80%-90%.The characteristic expanded in water using montmorillonite can make
It is separated with symbiosis nonmetallic mineral, then using the two granule size and density variation, is set by machineries such as eddy flow, centrifugations
It is standby, the thick non-clay mineral of particle is separated off, but granularity it is tiny and with the close symbiosis of montmorillonite α quartz and grain
Degree extremely tiny (0.1-0.5 μm) inlays alpha cristobalite together with montmorillonite, only relies on the hydration swelling power of montmorillonite itself
It is still not enough to open the symbiosis between three, inlays, package situation, particularly the high calcium-base bentonite of layer charge, therefore, it is impossible to
Removing is isolated with common hydraulic vortex flow devices, becomes the principal element and Montmorillonite Purification for influencing Montmorillonite Purification quality
The difficult point of technology.
It is also very universal to the research of the purifying process of montmorillonite, as the patent document of Patent No. CN1803607A discloses
A kind of preparation method of high-purity montmorillonite, but this method achievees the effect that separate montmorillonite using chemical reagent is added in, and causes
Montmorillonite contains substantial amounts of harmful chemical, and the montmorillonite purified is not suitable for being applied to medicine and food service industry.
The patent document of Patent No. CN101049940A discloses a kind of method for purifying superfine montmorillonite, and this method is in life
It produces in montmorillonite technical process, each production stage does not state the control of the intermediate of technological parameter and material in each link
Index, so that technique is unable to control during production, the montmorillonite quality for causing output is unstable, does not state going out for material particularly
Bacterium method can not be used in medicine and food service industry.
A kind of superfine montmorillonite purification disclosed in 17 days June in 2009 of the patent of invention of Patent No. CN100500563
Method, is delaminated by ultra-fine, and the reunion for effectively opening montmorillonite and impure mineral is wrapped up, and improves the scattered suspension of montmorillonite
Performance is conducive to further processing；It is classified simultaneously using its difference of specific gravity, but also is difficult to reach food grade mark
It is accurate.
The content of the invention
An object of the present invention is to provide a kind of food-grade montmorillonite, and degree of purification is high, and adsorption capacity is strong, meets medicine
With the requirement of food service industry；
It is low for equipment requirements, production cost is low the second object of the present invention is to provide the preparation process of food-grade montmorillonite,
Purification effect is good, is suitble to large-scale production.
In order to achieve the above object, the present invention adopts the following technical scheme that：Food-grade montmorillonite, purity be more than 99.0%,
Heavy metal lead is less than 5ppn, whiteness is more than 80%, cation exchange capacity and is more than 120mmol/100g.
The preparation process of food-grade montmorillonite, includes the following steps：（1）Montmorillonite raw material is dried under the conditions of 70-90 DEG C
Afterwards, 300-500 mesh is crushed to, obtains raw material powder；（2）Water is added in into raw material powder, is stirred and evenly mixed with raw material powder, obtained solid content is
The slurries of 10-25%；（3）The slurries cross 400-500 mesh sieves, obtain the first filtrate；（4）First filtrate be sent into ultra-fine equipment into
Row is ultra-fine to delaminate, and removes solid particle using classifying equipoment after delaminating, obtains the second filtrate；（5）Second filtrate is gone out
Bacterium, concentration, drying obtain food-grade montmorillonite product.
The technical solution is made by crushing, slurrying, coarse filtration, fine filtering, sterilizing series of steps in color and luster, purity, absorption
The parameters such as ability reach the montmorillonite product of food-grade requirement, and product quality is stablized, and entire technical process is at low cost, can advise greatly
Mould produces.
Preferably, step（1）Obtained raw material powder, first passes through pre-treatment, according still further to step（2）Operation, before described
Processing step is as follows：Raw material powder is added in sodium salt solution, when processing 2-5 is small, filtering obtains treatment fluid；Raw material powder and sodium
The weight ratio of salting liquid is 1:1-3.
In nature, mainly based on ca-montmorillonite, after being dispersed in water, though individual particle has slight expansion,
State is still kept building up between crystal grain so that be embedded in the granulometric impurities such as cristobalite therein and be wrapped wherein, can not isolate
Come, pre-treatment is carried out to it using sodium salt, the crystal layer of montmorillonite can be further opened, release impurity therein, so
Carry out subsequent purification processes again afterwards, obtained montmorillonite purity higher.
Preferably, the treatment temperature of pre-treatment is 70-90 DEG C, temperature directly affects point of the sodium salt in montmorillonite raw material
It dissipates, temperature is higher, scattered more abundant, but temperature is excessively high, can influence the concentration of montmorillonite raw material powder solution, and can limit sodium salt
It is scattered, it is selected in 70-90 DEG C most preferably.
Preferably, adding in zeolite in the treatment fluid that pre-treatment obtains, in mixing plant, when stir process 1-3 is small, stir
Speed is mixed as 200-300 revs/min.
Zeolite can be with heavy metal present in adsorption treatment liquid, especially heavy metal lead, moreover it is possible to it decolourizes to treatment fluid,
With above-mentioned rotating speed stir process 1-3 it is small when, heavy metal contaminants are fallen in fully absorption, ensure the security of montmorillonite product, carry
The whiteness of high product.
Preferably, the grain size of the zeolite is 0.1-0.3mm, adsorption effect is optimal.
Preferably, mixture of the sodium salt for one or more of sodium carbonate or sodium acid carbonate or sodium pyrophosphate,
The concentration of sodium salt is 50-80%.
Above-mentioned sodium salt is good to the opening effect of montmorillonite crystal layer, and cost is also low,
Preferably, the sodium salt is sodium carbonate and the mixture of sodium pyrophosphate, mass mixing ratio 3-5:1.
Preferably, step（2）While middle addition water, be also added into raw material powder weight 0.01-0.1% it is scattered
Agent, the dispersant are calgon, sodium trimetaphosphate, weight sodium metaphosphate, sodium carbonate, sodium acid carbonate, waterglass or burnt phosphorus
One or more of sour sodium mixture.
Preferably, after the sterilizing of the second filtrate, acidification is carried out, then carries out subsequent concentration, drying, obtains food-grade
Montmorillonite product.Acidification is carried out by the surface to montmorillonite, changes the activation energy on its surface, it is de- greatly to improve illiteracy
The exchange capacity of stone.
Implement said program, the present invention：By being suitble to the technique of large-scale production, simple equipment and step, system are utilized
For going out, purity is high, adsorption capacity is strong, whiteness is high, can reach the green montmorillonite product of food grade.
Specific embodiment
With reference to specific embodiment, the present invention is described in further detail.
Embodiment 1：
The preparation process of food-grade montmorillonite, includes the following steps：（1）After montmorillonite raw material being dried under the conditions of 90 DEG C,
Moisture content is no more than 5%, and the present embodiment is preferably 3%, is crushed to 300 mesh, obtains raw material powder；（2）Water is added in into raw material powder, with original
Feed powder stirs and evenly mixs, and the slurries that solid content is 10% are made；（3）The slurries cross 450 mesh sieves, obtain the first filtrate；（4）First filter
Liquid be sent into ultra-fine equipment carry out it is ultra-fine delaminate, remove solid particle using classifying equipoment after delaminating, obtain the second filtrate；
（5）By second filtrate sterilizing, concentration, drying, food-grade montmorillonite product, the purity 99.5% of montmorillonite, heavy metal are obtained
Lead 4.5ppn, whiteness 82%, cation exchange capacity 123mmol/100g.
Embodiment 2：
The preparation process of food-grade montmorillonite, includes the following steps：（1）Montmorillonite raw material is dried under the conditions of 70 DEG C to containing
After water rate is 5%, 400 mesh are crushed to, obtain raw material powder；（2）Pre-treatment is carried out to obtained raw material powder, step is as follows：By concentration
It is added to for 50% sodium salt solution in raw material powder, when processing 3 is small under conditions of temperature is 70 DEG C, filtering obtains treatment fluid；
Processing powder is obtained after treatment fluid concentration, drying；Sodium salt is the mixture of sodium carbonate and sodium pyrophosphate, mass mixing ratio 3:1；It is former
Feed powder and the weight ratio of sodium salt solution are 1:1；（3）Water and dispersant are added in into processing powder, is stirred and evenly mixed with raw material powder, is made
Solid content is 25% slurries；Dispersant is the 0.05% of raw material powder weight, selects calgon；（4）The slurries mistake
500 mesh sieves obtain the first filtrate；（5）First filtrate be sent into ultra-fine equipment carry out it is ultra-fine delaminate, using classifying equipoment after delaminating
Solid particle is removed, obtains the second filtrate；（6）By second filtrate sterilizing, concentration, drying, the production of food-grade montmorillonite is obtained
Product, purity 99.3%, heavy metal lead 3ppn, whiteness 86%, cation exchange capacity 150mmol/100g.
Embodiment 3：
The preparation process of food-grade montmorillonite, includes the following steps：（1）Montmorillonite raw material is dried under the conditions of 80 DEG C to containing
After water rate is 4%, after, 500 mesh are crushed to, obtain raw material powder；（2）Pre-treatment is carried out to obtained raw material powder, step is as follows：It will
The sodium salt solution that concentration is 70% is added in raw material powder, and when processing 5 is small under the conditions of at a temperature of 90 °C, filtering is handled
Liquid；The zeolite that grain size is 0.2mm is added in treatment fluid, in mixing plant, when stir process 2 is small, mixing speed 200
Rev/min, it then concentrates, processing powder is obtained after spray drying；Sodium salt is sodium carbonate；The weight ratio of raw material powder and sodium carbonate liquor
For 1:2；（3）Water and 00.1% dispersant of raw material powder weight are added in into processing powder, is stirred and evenly mixed with raw material powder, is made solid
Content is 20% slurries；The dispersant is sodium pyrophosphate；（4）The slurries cross 400 mesh sieves, obtain the first filtrate；（5）First
Filtrate be sent into ultra-fine equipment carry out it is ultra-fine delaminate, using solid particle is removed in classifying equipoment centrifuge after delaminating, obtain
Second filtrate；（6）To ultrasound sterilizing under the second filtrate high-temperature and high-pressure conditions, after acid treatment is carried out to it, concentration, spraying are dry
It is dry, food-grade montmorillonite product is obtained, purity 99.6%, heavy metal lead 3ppn, whiteness 87%, cation exchange capacity are
155mmol/100g。
Embodiment 4：
The preparation process of food-grade montmorillonite, includes the following steps：（1）Montmorillonite raw material is dried under the conditions of 80 DEG C to containing
After water rate is 4.5%, after, 500 mesh are crushed to, obtain raw material powder；（2）Pre-treatment is carried out to obtained raw material powder, step is as follows：
The sodium salt solution of concentration 80% is added in raw material powder, when processing 5 is small under the conditions of at a temperature of 90 °C, filtering is handled
Liquid；The zeolite that grain size is 0.3mm is added in treatment fluid, in mixing plant, when stir process 1.5 is small, mixing speed 250
Rev/min, it then concentrates, processing powder is obtained after spray drying；Sodium salt is the mixture of sodium carbonate and sodium pyrophosphate, mass mixing
Than for 5:1；The weight ratio of raw material powder and sodium salt solution is 1:2；（3）The 0.01% of water and raw material powder weight is added in into processing powder
Dispersant, stirred and evenly mixed with raw material powder, be made solid content be 20% slurries；The dispersant is calgon and burnt phosphorus
Sour sodium in mass ratio 1:2 mixture；（4）The slurries cross 400 mesh sieves, obtain the first filtrate；（5）First filtrate is sent into ultra-fine set
Standby middle progress is ultra-fine to delaminate, and using solid particle is removed in classifying equipoment centrifuge after delaminating, obtains the second filtrate；（6）It is right
Ultrasound sterilizing under second filtrate high-temperature and high-pressure conditions, after acid treatment is carried out to it, concentration, spray drying obtain food-grade
Montmorillonite product, purity 99.8%, heavy metal lead 1ppn, whiteness 80%, cation exchange capacity 180mmol/100g.
Embodiment 5：
The preparation process of food-grade montmorillonite, includes the following steps：（1）Montmorillonite raw material is dried under the conditions of 85 DEG C to containing
After water rate is 3%, after, 450 mesh are crushed to, obtain raw material powder；（2）Pre-treatment is carried out to obtained raw material powder, step is as follows：It will
The sodium salt solution that concentration is 60% is added in raw material powder, and when processing 4 is small under conditions of temperature is 80 DEG C, filtering is handled
Liquid；The zeolite that grain size is 0.2mm is added in treatment fluid, in mixing plant, when stir process 1 is small, mixing speed 300
Rev/min, it then concentrates, processing powder is obtained after spray drying；Sodium salt is the mixture of sodium carbonate and sodium pyrophosphate, mass mixing
Than for 4:1；The weight ratio of raw material powder and sodium salt solution is 1:3；（3）The 0.08% of water and raw material powder weight is added in into processing powder
Dispersant, stirred and evenly mixed with raw material powder, be made solid content be 20% slurries；The dispersant is sodium trimetaphosphate；（4）Institute
It states slurries and crosses 400 mesh sieves, obtain the first filtrate；（5）First filtrate be sent into ultra-fine equipment carry out it is ultra-fine delaminate, after delaminating using
Solid particle is removed in classifying equipoment centrifuge, obtains the second filtrate；（6）It is gone out to the second filtrate with ultrasound under high-temperature and high-pressure conditions
Bacterium, after acid treatment is carried out to it, concentration, spray drying obtain food-grade montmorillonite product, purity 99.9%, heavy metal lead
For 0ppn, whiteness 90%, cation exchange capacity 200mmol/100g.
Claims (3)
1. a kind of preparation process of food-grade montmorillonite, includes the following steps：（1）It is former that montmorillonite is dried under the conditions of 70-90 DEG C
After material, 300-500 mesh is crushed to, obtains raw material powder；（2）Water is added in into raw material powder, is stirred and evenly mixed with raw material powder, solid content is made
For the slurries of 10-25%；（3）The slurries cross 400-500 mesh sieves, obtain the first filtrate；（4）First filtrate is sent into ultra-fine equipment
Carry out it is ultra-fine delaminate, after delaminating using classifying equipoment remove solid particle, obtain the second filtrate；（5）By second filtrate
Sterilizing, concentration, drying, obtain food-grade montmorillonite product；Step（1）Obtained raw material powder, first passes through pre-treatment, according still further to
Step（2）Operation, the pre-treatment step are as follows：Raw material powder is added in sodium salt solution, when processing 2-5 is small, filtering obtains
Treatment fluid；The weight ratio of raw material powder and sodium salt solution is 1:1-3；The treatment temperature of the pre-treatment is 70-90 DEG C；Pre-treatment obtains
To treatment fluid in add in zeolite, in mixing plant, when stir process 1-3 is small, mixing speed be 200-300 revs/min；Institute
The grain size for stating zeolite is 0.1-0.3mm；The sodium salt is one or more of sodium carbonate or sodium acid carbonate or sodium pyrophosphate
Mixture, the concentration of sodium salt is 50-80%；The purity of the montmorillonite is more than 99.0%, heavy metal lead and is more than less than 5ppn, whiteness
80%th, cation exchange capacity is more than 120mmol/100g.
2. the preparation process of food-grade montmorillonite according to claim 1, it is characterised in that：Step（2）It is middle to add in the same of water
When, be also added into the dispersant of the 0.01-0.1% of raw material powder weight, the dispersant is calgon, sodium trimetaphosphate,
One or more of weight sodium metaphosphate, sodium carbonate, sodium acid carbonate, waterglass or sodium pyrophosphate mixture.
3. the preparation process of food-grade montmorillonite according to claim 1, it is characterised in that：After the sterilizing of second filtrate, carry out
Acidification, then subsequent concentration, drying are carried out, obtain food-grade montmorillonite product.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0360423A (en) * | 1989-07-26 | 1991-03-15 | Agency Of Ind Science & Technol | Heat resistant alumina cross-linked montmorillonite and production thereof |
| CN101049940A (en) * | 2007-03-29 | 2007-10-10 | 浙江三鼎科技有限公司 | Method for purifying superfine montmorillonite |
| CN101340979B (en) * | 2006-02-09 | 2010-06-16 | 浙江海力生制药有限公司 | Method for purifying montmorillonite, purified montmorillonite and combination thereof |
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- 2015-08-14 CN CN201510496004.8A patent/CN105016352B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0360423A (en) * | 1989-07-26 | 1991-03-15 | Agency Of Ind Science & Technol | Heat resistant alumina cross-linked montmorillonite and production thereof |
| CN101340979B (en) * | 2006-02-09 | 2010-06-16 | 浙江海力生制药有限公司 | Method for purifying montmorillonite, purified montmorillonite and combination thereof |
| CN101049940A (en) * | 2007-03-29 | 2007-10-10 | 浙江三鼎科技有限公司 | Method for purifying superfine montmorillonite |
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