CN109774001A - A kind of preparation method of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane - Google Patents
A kind of preparation method of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane Download PDFInfo
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- CN109774001A CN109774001A CN201811423646.5A CN201811423646A CN109774001A CN 109774001 A CN109774001 A CN 109774001A CN 201811423646 A CN201811423646 A CN 201811423646A CN 109774001 A CN109774001 A CN 109774001A
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- calcium carbonate
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Abstract
The invention discloses the preparation methods of a kind of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane, the equipment includes feeder, first plasticization portion, generate high steam portion, second plasticization portion and de-watering section, feeder, first plasticization portion, generate high steam portion, second plasticization portion and de-watering section are sequentially connected logical, it generates high steam portion and is equipped with the regulator for being used to adjust internal pressure, dewatering part is intermediate pressure section, normal pressure section and negative pressure section, intermediate pressure section, the regulator for adjusting internal pressure is equipped in normal pressure section and negative pressure section, preparation method is that will be put into batch mixer to mix with other ingredients again after nanometer calcium carbonate filter-press dehydration, it is finally putting into progress high temperature hydration in high temperature hydrating apparatus, it is finally putting into granulating and forming in pelletizer.The present invention has broken secondary agglomeration caused by nanometer calcium carbonate elder generation crushed after being dried classification process, forms drying, mixes, is granulating integrated.
Description
Technical field
The present invention relates to nanometer calcium carbonate technical fields, and in particular to a kind of high temperature hydrating apparatus and a kind of transparent membrane are special
With the preparation method of high filler loading capacity nanometer calcium carbonate master batch.
Background technique
Currently, the preparation method about nm level CaCO_3 has very much, calcium carbonate preparation method is divided into liquid phase reactor method and carbonization
Method.Liquid phase reactor method is to prepare calcium carbonate, gained by reaction between two kinds of solution of calcium salt and polcarb or bicarbonate
The most of patterns of product are relatively regular and particle size is micron order, and the reaction volume used due to it is few and preparation process is difficult
With the limitation of control, it is difficult to application of being magnified.Carbonizatin method is the main method of current industrial production nanometer calcium carbonate, should
Method raw material sources are extensive, and primary raw material is by selected lime stone.Lime stone obtains CaO by calcining；Then by CaO digestion
It is passed through CO2, chemical additives are added, carbonization is to terminal；Final product was waited by surface treatment, dehydration, drying, crushing and classification
Journey obtains nano-calcium carbonate calcium product.
In the preparation process of nanometer calcium carbonate, due to the most diverse of the surface property of its each material, it usually needs make
Powder body material particle surface is infiltrated, coated or generated with the resin of surface treating agent either high melt flow rate (MFR)
The coupling of chemical reaction.Since various powder body material surface performances have feature, often it is not achieved expected effect, and due to
Moisture cannot be completely exhausted out when dry, easily caused the defect inside nanometer calcium carbonate, influenced its mechanical property.
Summary of the invention
Problem to be solved by this invention is: providing a kind of high temperature hydrating apparatus and a kind of dedicated high filler loading capacity of transparent membrane
The preparation method of nanometer calcium carbonate master batch is to solve the problems, such as the defect of the inside occurred in the preparation process of nanometer calcium carbonate.
The present invention in order to solve the above problem provided by technical solution are as follows: a kind of high temperature hydrating apparatus, including feeder, the
One plasticization portion generates high steam portion, the second plasticization portion and de-watering section, and the feeder, generates height at the first plasticization portion
Steam portion, the second plasticization portion and de-watering section is pressed to be sequentially connected logical, the feeder upper end is equipped with feed inlet, the generation high pressure
Steam portion is equipped with the regulator for being used to adjust internal pressure, and the dewatering part is intermediate pressure section, normal pressure section and negative pressure section, institute
The regulator being equipped on intermediate pressure section, normal pressure section and negative pressure section for adjusting internal pressure is stated, the de-watering section is far from described
The one end in the second plasticization portion is equipped with taking-up portion.
A kind of preparation method of the dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane, includes the following steps,
The nanometer calcium carbonate crystal that diameter is 20-30nm is carried out filter-press dehydration by step 1), and forming water content is 40%
Nanometer calcium carbonate filter cake；
Step 2), by aqueous 40% nanometer calcium carbonate filter cake, polyethylene, PE wax, stearic acid, calcium stearate, PETS and
Coupling agent is put into high speed mixer and is mixed, and weight percent is nanometer calcium carbonate filter cake 83%, polyethylene 12%, PE wax
2%, stearic acid 0.7%, calcium stearate 0.7%, PETS0.35% and coupling agent 0.35%；
The material mixed from the step 2) is put into high temperature hydrating apparatus as described in claim 1 by step 3)
Middle progress high temperature hydration；
Material after being hydrated from step 3) high temperature is put into granulating and forming in pelletizer by step 4), is finally made saturating
The bright dedicated high filler loading capacity nanometer calcium carbonate master batch of film.
Preferably, the coupling agent in the step 3) be titanate esters, it is silane, phosphate, borate, any in Aluminate
It is a kind of.
Preferably, the mixing temperature in the step 3) is 120 DEG C, incorporation time 4h.
Compared with prior art, the invention has the advantages that the present invention by using coupling agent nanometer calcium carbonate production
Synergistic effect is played in the process, improves the binding force of high nanometer calcium carbonate and resin；Meanwhile by polyphosphazene polymer olefin resin material
Material is merged with aqueous nanometer calcium carbonate filter cake, in the process moisture evaporation；Nanometer calcium carbonate elder generation crushed after being dried point is broken
Secondary agglomeration caused by during grade forms drying, mixes, is granulating integrated.
Detailed description of the invention
The drawings described herein are used to provide a further understanding of the present invention, constitutes a part of the invention, this hair
Bright illustrative embodiments and their description are used to explain the present invention, and are not constituted improper limitations of the present invention.
Fig. 1 is the schematic diagram of high temperature hydrating apparatus of the invention；
Attached drawing mark: 1, feed inlet, 2, regulator, 3, taking-up portion, 4, negative pressure section, 5, normal pressure section, 6, de-watering section, 7,
Intermediate pressure section, the 8, second plasticization portion, 9, generation high steam portion, the 10, first plasticization portion, 11, feeder.
Specific embodiment
Carry out the embodiment that the present invention will be described in detail below in conjunction with accompanying drawings and embodiments, how the present invention is applied whereby
Technological means solves technical problem and reaches the realization process of technical effect to fully understand and implement.
As shown in Figure 1, a kind of high temperature hydrating apparatus, including feeder 10, the first plasticization portion, generate high steam portion,
Second plasticization portion 8 and de-watering section 6, the feeder 11, generate high steam portion 9, the second plasticization at first plasticization portion 10
Portion 8 and de-watering section 6 are sequentially connected logical, and 11 upper end of feeder is equipped with feed inlet 11, sets in the generation high steam portion 9
Have a regulator 2 for adjusting internal pressure, the de-watering section 6 is divided for intermediate pressure section 7, normal pressure section 5 and negative pressure section 4, it is described in
The regulator 2 for adjusting internal pressure is equipped on pressure section 7, normal pressure section 5 and negative pressure section 4, the de-watering section 6 is far from institute
The one end for stating the second plasticization portion 8 is equipped with taking-up portion 3.
A kind of preparation method of the dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane, includes the following steps,
The nanometer calcium carbonate crystal that diameter is 20-30nm is carried out filter-press dehydration by step 1), and forming water content is 40%
Nanometer calcium carbonate filter cake；
Step 2), by aqueous 40% nanometer calcium carbonate filter cake, polyethylene, PE wax, stearic acid, calcium stearate, PETS and
Coupling agent is put into high speed mixer and is mixed, and weight percent is nanometer calcium carbonate filter cake 83%, polyethylene 12%, PE wax
2%, stearic acid 0.7%, calcium stearate 0.7%, PETS0.35% and coupling agent 0.35%；
The material mixed from the step 2) is put into high temperature hydrating apparatus as described in claim 1 by step 3)
Middle progress high temperature hydration, that is to say, that the material after mixing from step 2) is put into the feeder of high temperature mixing apparatus, so
Material carries out spiral plasticizing in the first plasticization portion afterwards, and then into generating in high steam portion, high pressure is mixed into material
Steam, the material for being then mixed with high steam enter in the second plasticization portion progress spiral plasticizing, enter back into de-watering section into
Row dehydration, finally takes out from taking-up portion.
Material after being hydrated from step 3) high temperature is put into granulating and forming in pelletizer by step 4), is finally made saturating
The bright dedicated high filler loading capacity nanometer calcium carbonate master batch of film.
Coupling agent in the step 3) is titanate esters, silane, phosphate, borate, any one in Aluminate.
Mixing temperature in the step 3) is 120 DEG C, incorporation time 4h.
The structure of the dedicated high filler loading capacity nanometer calcium carbonate master batch of the transparent membrane is made of four parts.
(1), innermost layer is filler core, i.e. nanometer calcium carbonate；Main rise improves rigidity, reduces the effects of cost；
(2), the second layer is coupling layer, is made of coupling agent or crosslinking agent, it is therefore an objective to improve nanometer calcium carbonate and resin
Binding force.The selection of coupling layer: it is generally coated using coupling agents such as titanate esters, silane, phosphate, borate, Aluminates
Processing, general dosage are the 0.5%~3% of amount of filler, sometimes for synergistic effect is played, suitably plus such as double Malaya of a little crosslinking agents
Amine, another to handle uniformly to improve synergistic effect, a little diluents of Chang Zaijia, such as ethyl alcohol, toluene, the effect for coating coupling agent
Fruit is more preferable；
(3), third layer is dispersion layer, is made of some oligomer and dispersing agent, it is therefore an objective to be uniformly mixed, avoid filler poly-
Collection improves mobility in granulation process.The selection of dispersion layer: stearic acid, stearate, low molecular weight polyethylene, low is generally selected
Molecular weight polystyrene and other low-molecular weight polymers, dosage is generally within 5%；
(4), the 4th layer, i.e. outermost layer is to increase mixed layer, by with certain double bond copolymer or compatibility agent form, it is therefore an objective to
It can preferably be combined with the resin to be filled.Increase the selection of mixed layer: generally multi-purpose random polypropylene (APP), softening point is low, packet
It is good to cover filler effect, also useful other resins such as LDPE, HDPE, LLDPE, PS, CPE, EVA etc., can be selected above-mentioned resin sometimes
Blend make vector resin, if LDPE and LLDPE are blended, synergy is good.If master batch is used for polyvinyl chloride resin, AMS may be selected
For resin as master batch carrier, filling effect is preferable.In addition to this, anhydrous maleic acid acid anhydride grafted polyethylene, polypropylene etc. also can be used
Filler is handled, effect is also fine.Increasing mixed layer dosage is 15% -30%.
(the performance rating standard of plastic master batch, is usually compareed with standard sample, such as color masterbatch for the performance rating of master batch
Grain.It is sometimes compared from following some aspects).
1, appearance color: apparent size size, is cylinder particle or rectangular particle, whiteness size, whether impurity in color.
2, moisture content and its fugitive constituent: it should be less than a certain numerical value, be such as defined as 0.2% -0.3%.
3, density: such as 1.7-1.9g/ml.
4, melt flow rate (MFR): it should be greater than a certain numerical value, be such as set to 0.5g/10min.
5, specific professional pointer: as what grade fire-retardant master granule should indicate flammability up to, such as UL-94V-0 grade, containing halogen quantity.
6, additive amount: 10% -15%, 30% -40% is such as added.
7, wherein it is important that processing and forming pointer, i.e. melt flow rate (MFR) and professional pointer.
Master-batch techniques pointer is general are as follows: density 1.7g/ml, moisture 0.2%, 0.5-10g/10min of melt flow rate (MFR),
Granule size 334mm.
The beneficial effects of the present invention are: the present invention plays in the manufacturing process of nanometer calcium carbonate by using coupling agent
Synergistic effect, improves the binding force of high nanometer calcium carbonate and resin；Meanwhile by macromolecule polyolefin material and aqueous nanometer
Calcium carbonate filter cake is merged, in the process moisture evaporation；Break in nanometer calcium carbonate elder generation crushed after being dried classification process and has caused
Secondary agglomeration, formed it is dry, mix, be granulating integrated.
Only highly preferred embodiment of the present invention is described above, but is not to be construed as limiting the scope of the invention.This
Invention is not only limited to above embodiments, and specific structure is allowed to vary.All protection models in independent claims of the present invention
Interior made various change is enclosed to all fall in the scope of protection of the present invention.
Claims (4)
1. a kind of high temperature hydrating apparatus, it is characterised in that: including feeder, the first plasticization portion, generate high steam portion, second
Plasticization portion and de-watering section, the feeder, generate high steam portion, the second plasticization portion and de-watering section at the first plasticization portion
It is sequentially connected logical, the feeder upper end is equipped with feed inlet, and the generations high steam portion is equipped with for adjusting internal pressure
Regulator, the dewatering part is intermediate pressure section, normal pressure section and negative pressure section, on medium pressure section, normal pressure section and negative pressure section
Equipped with the regulator for being used to adjust internal pressure, the de-watering section is equipped with far from the one end in second plasticization portion and takes out
Portion.
2. a kind of preparation method of the dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane, it is characterised in that: including following step
Suddenly,
The nanometer calcium carbonate crystal that diameter is 20-30nm is carried out filter-press dehydration by step 1), forms the nanometer that water content is 40%
Calcium carbonate filter cake；
Step 2), by aqueous 40% nanometer calcium carbonate filter cake, polyethylene, PE wax, stearic acid, calcium stearate, PETS and coupling
Agent is put into high speed mixer and is mixed, weight percent be nanometer calcium carbonate filter cake 83%, polyethylene 12%, PE wax 2%,
Stearic acid 0.7%, calcium stearate 0.7%, PETS0.35% and coupling agent 0.35%；
Step 3), from the material mixed in the step 2) be put into high temperature hydrating apparatus as described in claim 1 into
The hydration of row high temperature；
Material after being hydrated from step 3) high temperature is put into granulating and forming in pelletizer by step 4), and thin transparent is finally made
The dedicated high filler loading capacity nanometer calcium carbonate master batch of film.
3. a kind of preparation method of the dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane according to claim 2,
Be characterized in that: coupling agent in the step 3) is titanate esters, silane, phosphate, borate, any one in Aluminate.
4. a kind of preparation method of the dedicated high filler loading capacity nanometer calcium carbonate master batch of transparent membrane according to claim 2,
Be characterized in that: the mixing temperature in the step 3) is 120 DEG C, incorporation time 4h.
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Application publication date: 20190521 |