CN108530687A - One kind is for high whiteness calcium silicates and preparation method in plastic filler - Google Patents
One kind is for high whiteness calcium silicates and preparation method in plastic filler Download PDFInfo
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- CN108530687A CN108530687A CN201810378577.4A CN201810378577A CN108530687A CN 108530687 A CN108530687 A CN 108530687A CN 201810378577 A CN201810378577 A CN 201810378577A CN 108530687 A CN108530687 A CN 108530687A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses one kind for high whiteness calcium silicates and preparation method in plastic filler.The high whiteness calcium silicates is made by following steps：A, by calcium silicates, water and dispersant, it is made into slurry；B, high speed ball milling is carried out to slurry, calcium silicate particle surface is made fully to activate；C, aluminum nitrate solution is added in calcium silicates slurry and is mixed, ammonium hydroxide is added and is stirred to react, one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface after standing；D, the calcium silicates of high whiteness is made in filtering, drying.The method has the advantages that：The present invention to calcium silicates by first carrying out surface active, it uses aluminium salt and ammonium hydroxide to carry out liquid deposition again, has coated one layer of aluminium hydroxide sedimentary on calcium silicates surface, be remarkably improved the whiteness of calcium silicates, and preparation process is simple, can be extensively with the filling-modified field such as remaining plastics, rubber.
Description
Technical field
The present invention relates to plastic filler fields, and in particular to the preparation of calcium silicates is filled out more particularly, to one kind for plastics
Fill high whiteness calcium silicates and preparation method in masterbatch.
Background technology
With riseing for world petroleum price, cost is reduced using inorganic nonmetal mineral fillers in plastic products and moulded
Have great importance in material products production.Meanwhile the addition of inorganic non-metallic filler, plastic product mechanical performance is improved,
It even also assigns plastic product some special functions, such as the rigidity, hardness, dimensional stability of plastics can be improved.People
Common inorganic filler includes calcium carbonate, mica, wollastonite, talcum, kaolin, silica, titanium dioxide, calcium sulfate.Nothing
Effect of the machine nonmetal mineral fillers in polymer composites sums up and is exactly increment, enhancing and assigns new function.
In inorganic filler, calcium silicate micro power is last century the seventies by a kind of new filler and thermal insulation separation of Japan's exploitation
Hot material mostly uses hydrothermal synthesis method preparation, is a kind of new inorganic material that market scale increases year by year.Using sodium metasilicate
The technique that solution dissolves milk of lime can also produce calcium silicate micro power, but the recycling difficulty of lye is very big.So to inorganic non-
Metalliferous mineral filler is modified, and improves its intermiscibility with organic polymer, avoids stress dispersion caused by directly adding not
.Preparation method half grease thermal synthesis method, the sodium silicate solution of calcium carbonate dissolve the technique etc. of milk of lime at present.
Number of patent application 201610055080.X discloses a kind of low ph value high oil absorption value and specific surface area calcium silicate powder
Preparation method comprising following steps：（1）Emulsification pretreatment obtains calcium hydroxide suspension after calcium hydroxide adds water；（2）Hydrogen-oxygen
Change calcium hanging drop and is added to generation calcium silicates slurry in the sodium silicate solution of sodium silicate solution or aluminum contained compound；（3）Calcium silicates
After slurry filters, gained filter cake adds water emulsification pretreatment to obtain dealkalize calcium silicates slurry；（4）Acidic silicate solution is added drop-wise to dealkalize
The calcium silicates suspension that pH value is 9 ~ 11 is formed in calcium silicates slurry, then washed, drying obtains low ph value calcium silicate powder.It should
Powder has the characteristics that low ph value, high whiteness, high oil absorption value, high-specific surface area, can be used as the matrixes material such as rubber, plastics, paper
The filler of material improves the mechanical property of basis material.
Number of patent application 201710984760.4 discloses a kind of preparation method of hydrated calcium silicate, includes the following steps：
（1）The mixed liquor of sodium silicate solution, calcium nitrate solution and water three is placed in plastic containers and ultrasonic mixing, hydrogen-oxygen is then added
Change sodium solution, makes mixed solution pH ＞ 13；（2）Toward step（1）In plastic containers in be passed through after nitrogen excludes remaining air
Seal the plastic containers, then by plastic containers in ultrasonic container 15 ~ 30min of ultrasound, so that reactant is sufficiently mixed
It is even, uniformly mixed system is placed in constant water bath box, setting temperature is 20 ~ 100 DEG C, and the reaction time is 3 ~ 7d；（3）Instead
After answering, product washing, the filtering that step 2) is obtained are multiple, the foreign ion of removal surface remnants；（4）It will step
Suddenly（3）Obtained product is placed on vacuum drying chamber, and drying to constant weight to get to hydrated calcium silicate product.Water prepared by the invention
Change calcium silicates purity is high, single yield is big, preparation process is simple, has preferable application prospect.
Number of patent application 201710905712.1 disclose it is a kind of synthesis high activity, Lower alrali content calcium silicates producer
Method has been separately added into water repellent agent on the basis of 3 ~ 5 sections of washings of tradition in first segment washing dehydration and final stage washing dehydration
And de alkali additive, achieve the purpose that water-saving and efficient removal alkali, the water repellent agent being wherein added in first segment washing dehydration are alkaline-resisting
Property hydrophobic polymeric polymer, the aluminium ion in aluminium salt in the de alkali additive being added in final stage washing dehydration then can and silicon
Water and aluminum hydroxide precipitation is obtained by the reaction in sodium hydroxide in sour calcium, achievees the purpose that dealkalize；The preparation method of the invention operates
Simply, flexibly, there is no any influence to existing synthetic calcium silicate synthesis technology, without additional large scale equipment is increased, only need to increase
Add storage and the adding set of corresponding additive.Meanwhile the wash water consumption of synthetic calcium silicate can be greatly reduced in the invention, reduce life
Produce the discharge of the consumption of process water.
Number of patent application 201510184967.4 discloses a kind of method preparing ultra-fine high-brightness calcium silicate micro power, is alkali
It soaks low alumina-silicon ratio alumyte, aluminous fly-ash, calcining coal series kaolin rock spoil eka-aluminum material and solution of sodium metasilicate through is made, mode transfer adds
Add crystal seed, cooling, crystallization to remove the impurity for entering solution when alkali leaching, obtains pure non-hydrate sodium metasilicate or five water metasilicic acids
Sodium crystal.After crystal melt, supplying milk of lime carries out slurry reaction, prepares the silicon of whiteness >=94, average grain diameter≤20 μm
Sour calcium micro mist.Calcium silicate products purity prepared by the present invention, whiteness are high, and added value is high, can be widely applied to coating, rubber, modeling
Material and paper-making industry, also act as heat preserving and insulating material.
It can be seen that the preparation process of calcium silicates is complex in the prior art, and preparation mixing can not be effectively removed
The impurity such as alundum (Al2O3), titanium dioxide, di-iron trioxide in object, lead to that product purity is poor, whiteness is low, and then exist and influence
The problems such as application effect in calcium silicates filling plastic.
Invention content
Effectively to solve above-mentioned technical problem, the present invention proposes a kind of for high whiteness calcium silicates in plastic filler
And preparation method, the purity of calcium silicates can be effectively improved, and have fabulous whitening effect.
The specific technical solution of the present invention is as follows：
A kind of preparation method for high whiteness calcium silicates in plastic filler, the high whiteness calcium silicates is by surface
In the calcium silicates slurry fully activated, aluminum nitrate carries out liquid deposition with ammonium hydroxide, and one layer of aluminium hydroxide is coated on calcium silicates surface
Sedimentary, plays bridging effect to staining impurity substance in calcium silicates and is made, and specific preparation process is：
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, aluminum nitrate solution is added in calcium silicates slurry, is thoroughly mixed, is slowly added to ammonium hydroxide, continue to be stirred to react 2 ~
3h is then allowed to stand, and one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
D, the calcium silicates of high whiteness is made in filtering, drying.
Preferably, in the step a, dispersant is barium stearate, calcium stearate, zinc stearate, copper stearate or tristearin
At least one of sour magnesium.
Preferably, in the step a, 20 ~ 30 parts by weight of calcium silicates, 68 ~ 79 parts by weight of water, 1 ~ 2 parts by weight of dispersant.
Preferably, in the step a, pH value is 7 ~ 8.
Preferably, in the step b, the drum speed of high speed ball milling is 20 ~ 30r/min, and the time is 30 ~ 50min.
Preferably, in the step c, 15 ~ 20 parts by weight of aluminum nitrate, 54 ~ 63 parts by weight of calcium silicates slurry, ammonium hydroxide 22 ~ 26
Parts by weight.
Preferably, in the step c, time of repose is 3 ~ 5h.
Preferably, in the step d, dry heating temperature is 120 ~ 130 DEG C, and the time is 40 ~ 60min.
Surface active is carried out to calcium silicates, by different piece in molecule respectively for the affine of two-phase, two-phase is made will
It regards the ingredient of this phase as, and molecules align between the two phases, makes the surface of two-phase be equivalent to and is transferred to intramolecule.To reduce table
Face tension.Since two-phase is all regarded as a component of this phase, being equivalent to two phases and surfactant molecule does not all have
Interface is formed, the interface of two phases of the elimination of part in this way is equivalent to, just reduces surface tension and surface
Free energy.Then aluminium hydroxide sedimentary is generated by the calcium silicates surface liquid deposition reaction in surface active, be evenly distributed
And be tightly combined with calcium carbonate, using the high whiteness characteristic of aluminium hydroxide sedimentary itself, cladding can be played and brighten calcium carbonate
Effect.
The above of the present invention also proposed it is a kind of for high whiteness calcium silicates in plastic filler, first to calcium silicates into
The high speed ball milling of row certain time activates, then carries out liquid deposition using aluminium salt and ammonium hydroxide, and one layer has been coated on calcium silicates surface
Aluminium hydroxide sedimentary plays bridging effect to staining impurity substance in calcium silicates, product whiteness is made to significantly improve.By packet
Cover the high quality filler that the calcium silicate products brightened is widely used as the fields such as plastics, rubber.
Beneficial effects of the present invention are：
Clad preparation is deposited for high whiteness silicon in plastic filler 1. proposing and generating aluminium hydroxide by liquid deposition
The method of sour calcium.
2. the present invention to calcium silicates progress surface active, then using aluminium salt and ammonium hydroxide by first carrying out liquid deposition, in silicon
Sour calcium surface has coated one layer of aluminium hydroxide sedimentary, is remarkably improved the whiteness of calcium silicates.
It, can be extensively with the filling-modified field such as remaining plastics, rubber 3. preparation process of the present invention is simple.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, aluminum nitrate solution is added in calcium silicates slurry, is thoroughly mixed, is slowly added to ammonium hydroxide, continues to be stirred to react 2h,
It is then allowed to stand, one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
D, the calcium silicates of high whiteness is made in filtering, drying.
In step a, dispersant is barium stearate.
In step a, 26 parts by weight of calcium silicates, 73 parts by weight of water, 1 parts by weight of dispersant；In step c, 18 weight of aluminum nitrate
Part, 58 parts by weight of calcium silicates slurry, 24 parts by weight of ammonium hydroxide.
In step a, pH value 7；In step b, the drum speed of high speed ball milling is 25r/min, time 40min；Step c
In, time of repose 4h；In step d, dry heating temperature is 125 DEG C, time 50min.
Embodiment 2
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, aluminum nitrate solution is added in calcium silicates slurry, is thoroughly mixed, is slowly added to ammonium hydroxide, continues to be stirred to react 3h,
It is then allowed to stand, one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
D, the calcium silicates of high whiteness is made in filtering, drying.
In step a, dispersant is calcium stearate.
In step a, 20 parts by weight of calcium silicates, 79 parts by weight of water, 1 parts by weight of dispersant；In step c, 15 weight of aluminum nitrate
Part, 63 parts by weight of calcium silicates slurry, 22 parts by weight of ammonium hydroxide.
In step a, pH value 8；In step b, the drum speed of high speed ball milling is 20r/min, time 50min；Step c
In, time of repose 3h；In step d, dry heating temperature is 120 DEG C, time 60min.
Embodiment 3
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, aluminum nitrate solution is added in calcium silicates slurry, is thoroughly mixed, is slowly added to ammonium hydroxide, continues to be stirred to react 2h,
It is then allowed to stand, one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
D, the calcium silicates of high whiteness is made in filtering, drying.
In step a, dispersant is zinc stearate.
In step a, 30 parts by weight of calcium silicates, 68 parts by weight of water, 2 parts by weight of dispersant；In step c, 20 weight of aluminum nitrate
Part, 54 parts by weight of calcium silicates slurry, 26 parts by weight of ammonium hydroxide.
In step a, pH value 7；In step b, the drum speed of high speed ball milling is 30r/min, time 30min；Step c
In, time of repose 5h；In step d, dry heating temperature is 130 DEG C, time 40min.
Embodiment 4
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, aluminum nitrate solution is added in calcium silicates slurry, is thoroughly mixed, is slowly added to ammonium hydroxide, continues to be stirred to react 3h,
It is then allowed to stand, one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
D, the calcium silicates of high whiteness is made in filtering, drying.
In step a, dispersant is copper stearate.
In step a, 22 parts by weight of calcium silicates, 76 parts by weight of water, 2 parts by weight of dispersant；In step c, 16 weight of aluminum nitrate
Part, 60 parts by weight of calcium silicates slurry, 24 parts by weight of ammonium hydroxide.
In step a, pH value 8；In step b, the drum speed of high speed ball milling is 22r/min, time 45min；Step c
In, time of repose 3.5h；In step d, dry heating temperature is 122 DEG C, time 55min.
Embodiment 5
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, aluminum nitrate solution is added in calcium silicates slurry, is thoroughly mixed, is slowly added to ammonium hydroxide, continues to be stirred to react 2h,
It is then allowed to stand, one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
D, the calcium silicates of high whiteness is made in filtering, drying.
In step a, dispersant is magnesium stearate.
In step a, 28 parts by weight of calcium silicates, 70 parts by weight of water, 2 parts by weight of dispersant；In step c, 18 weight of aluminum nitrate
Part, 57 parts by weight of calcium silicates slurry, 25 parts by weight of ammonium hydroxide.
In step a, pH value 7；In step b, the drum speed of high speed ball milling is 28r/min, time 35min；Step c
In, time of repose 4.5h；In step d, dry heating temperature is 128 DEG C, time 45min.
Comparative example 1
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, aluminum nitrate solution is added in calcium silicates slurry made from step a, is thoroughly mixed, is slowly added to ammonium hydroxide, continued
It is stirred to react 2h, is then allowed to stand, one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
C, the calcium silicates of high whiteness is made in filtering, drying.
In step a, dispersant is barium stearate.
In step a, 26 parts by weight of calcium silicates, 73 parts by weight of water, 1 parts by weight of dispersant；In step b, 18 weight of aluminum nitrate
Part, 58 parts by weight of calcium silicates slurry, 24 parts by weight of ammonium hydroxide.
In step a, pH value 7；In step b, time of repose 4h；In step c, dry heating temperature is 125 DEG C, when
Between be 50min.
Embodiment 1 is not ground activation to calcium silicates slurry so that the aluminium hydroxide of surface deposition is uneven, and whiteness carries
Rise unobvious.
Comparative example 2
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, by calcium silicates slurry, it is slowly added to ammonium hydroxide, continues to be stirred to react 2h, be then allowed to stand；
D, calcium silicates is made in filtering, drying.
In step a, dispersant is magnesium stearate.
In step a, 28 parts by weight of calcium silicates, 70 parts by weight of water, 2 parts by weight of dispersant；In step c, calcium silicates slurry 57
Parts by weight, 25 parts by weight of ammonium hydroxide.
In step a, pH value 7；In step b, the drum speed of high speed ball milling is 28r/min, time 35min；Step c
In, time of repose 4.5h；In step d, dry heating temperature is 128 DEG C, time 45min.
Comparative example 2 is not introduced into aluminium hydroxide.Calcium silicates surface whiteness is caused not promoted.
Calcium silicates made from above-described embodiment 1 ~ 5 and comparative example 1-2 tests whiteness, test characterization method or condition such as
Under：
Whiteness：Whiteness test experiment is carried out according to GB3978-83, calcium silicates 5g produced by the present invention is taken, using WSB-VI whiteness
Analysis analyzer is tested, and using diffusion illuminating vertical detection mode, a diameter of 120mm of globe of diffusion, measured hole is a diameter of
The wavelength of 20mm, spectral response range are 457mm, a diameter of 20mm of pelleting press, measure 5 whiteness values, calculate average value.
The results are shown in Table 1.
Table 1：
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example 1 | Comparative example 2 |
| Whiteness（%） | 94.1 | 93.8 | 92.2 | 90.8 | 94.3 | 86.6 | 75.2 |
Claims (9)
1. a kind of preparation method for high whiteness calcium silicates in plastic filler, it is characterised in that：The high whiteness silicic acid
Calcium is wrapped on calcium silicates surface by the way that in the calcium silicates slurry that surface fully activates, aluminum nitrate carries out liquid deposition with ammonium hydroxide
One layer of aluminium hydroxide sedimentary is covered, bridging effect is played to staining impurity substance in calcium silicates and is made, specific preparation process
For：
A, by calcium silicates, water and dispersant, it is made into slurry, and adjust pH value；
B, high speed ball milling is carried out to slurry made from step a, calcium silicate particle surface is made fully to activate；
C, aluminum nitrate solution is added in calcium silicates slurry, is thoroughly mixed, is slowly added to ammonium hydroxide, continue to be stirred to react 2 ~
3h is then allowed to stand, and one layer of aluminium hydroxide sedimentary is coated on calcium silicates surface by liquid deposition；
D, the calcium silicates of high whiteness is made in filtering, drying.
2. a kind of preparation method for high whiteness calcium silicates in plastic filler, feature exist according to claim 1
In：In the step a, dispersant be barium stearate, calcium stearate, zinc stearate, copper stearate or magnesium stearate at least
It is a kind of.
3. a kind of preparation method for high whiteness calcium silicates in plastic filler, feature exist according to claim 1
In：In the step a, 20 ~ 30 parts by weight of calcium silicates, 68 ~ 79 parts by weight of water, 1 ~ 2 parts by weight of dispersant.
4. a kind of preparation method for high whiteness calcium silicates in plastic filler, feature exist according to claim 1
In：In the step a, pH value is 7 ~ 8.
5. a kind of preparation method for high whiteness calcium silicates in plastic filler, feature exist according to claim 1
In：In the step b, the drum speed of high speed ball milling is 20 ~ 30r/min, and the time is 30 ~ 50min.
6. a kind of preparation method for high whiteness calcium silicates in plastic filler, feature exist according to claim 1
In：In the step c, 15 ~ 20 parts by weight of aluminum nitrate, 54 ~ 63 parts by weight of calcium silicates slurry, 22 ~ 26 parts by weight of ammonium hydroxide.
7. a kind of preparation method for high whiteness calcium silicates in plastic filler, feature exist according to claim 1
In：In the step c, time of repose is 3 ~ 5h.
8. a kind of preparation method for high whiteness calcium silicates in plastic filler, feature exist according to claim 1
In：In the step d, dry heating temperature is 120 ~ 130 DEG C, and the time is 40 ~ 60min.
9. one kind that any one of claim 1 ~ 8 the method is prepared is for high whiteness calcium silicates in plastic filler.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116731397A (en) * | 2023-07-20 | 2023-09-12 | 浙江钦堂钙业有限公司 | Modified shell-core structure calcium carbonate with flame retardant function |
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2018
- 2018-04-25 CN CN201810378577.4A patent/CN108530687A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116731397A (en) * | 2023-07-20 | 2023-09-12 | 浙江钦堂钙业有限公司 | Modified shell-core structure calcium carbonate with flame retardant function |
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