CN107674455A - A kind of calcium carbonate modifier and its method of modifying - Google Patents
A kind of calcium carbonate modifier and its method of modifying Download PDFInfo
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- CN107674455A CN107674455A CN201710763837.5A CN201710763837A CN107674455A CN 107674455 A CN107674455 A CN 107674455A CN 201710763837 A CN201710763837 A CN 201710763837A CN 107674455 A CN107674455 A CN 107674455A
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- calcium carbonate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The present invention relates to calcium carbonate modified technical field, especially a kind of calcium carbonate modifier and its method of modifying, after compound, odium stearate and urea phosphate progress compatibility, as calcium carbonate modified, be capable of high degree raising calcium carbonate make filler after, be prepared into the mechanical property of product, improve the quality that calcium carbonate is used as filler, solve in the prior art, calcium carbonate be used as filler be prepared into product mechanical property it is poor the defects of.
Description
Technical field
The present invention relates to calcium carbonate modified technical field, especially a kind of calcium carbonate modifier and its method of modifying.
Background technology
It is well known that calcium carbonate is to apply extremely wide inorganic filler, it may be used on plastics, rubber, coating, adhesive
Deng in product, especially nano-calcium carbonate, because its particle diameter is small, specific surface area is big, is added in matrix material, can be effective
The mechanical property and processing characteristics of material are improved, still, because calcium carbonate is bad there is compatibility with matrix resin, is easily sent out
It is raw to reunite, fault of construction is caused, causes the quality of product unstable, it is difficult to adapt to the demand in market, limit calcium carbonate product
Application.
At present, have for calcium carbonate surface inorganic agent it is a variety of, such as use coupling agent so that coupling agent one end is hydrophilic inorganic
The group of thing, firm chemical bond can be formed with the functional group reactionses of Nano particles of calcium carbonate；Other end is organophilic
Group, chemically reacted with polymer molecular chain, the presence of coupling agent is the larger material tight knot of two kinds of polarity spectrums
Altogether, realize that nanoparticle surface activity is obviously reduced, reduce reunion rate, improve dispersiveness in the base；Furthermore use
Aliphatic acid or soap surface are modified, and improve the compatibility with resin matrix；The third is with phosphate surface modified carbon acid
Calcium so that Compatibility improvement, strengthen the mechanical property of composite；4th kind is by polymer modification so that in surface shape
Film forming, improve its dispersiveness.
Although many to calcium carbonate modified method, still there are many limitations in it, and most of processing methods into
This is higher, and treatment effect is also undesirable, polymer modification described above, causes environmental pollution serious；Above-mentioned phosphate surface
Modified, it causes price higher；Aliphatic acid or soap are modified, such as stearic acid, although in calcium carbonate modified field
With higher cost performance, but because it is used cooperatively during modification, it is necessary to add substantial amounts of alkaline matter, lead
Particle surface pH value is caused to increase so that when applying in the polymer, it can be negatively affected, and hydroxy-acid group and calcium carbonate
Active force is weaker, it is difficult to calcium carbonate is realized uniformly modified so that local reunite easily occur.
In consideration of it, this researcher is studied for calcium carbonate modified with modifying agent, carried for calcium carbonate modified technical field
For a kind of NEW TYPE OF COMPOSITE modifying agent.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides a kind of calcium carbonate modifier and its changed
Property method.
It is achieved particular by following technical scheme：
Calcium carbonate modifier, material composition is in parts by weight compound 0.1-0.6 parts, odium stearate 0.001-0.007
Part, urea phosphate 0.01-0.06 parts；Wherein molecular structure of compounds is：
Wherein, R1 is one kind in phenyl, ether base, vinyl, cycloalkyl；R2 is methylene
One kind in base, ethylidene, CH2CH2CH2OCH2CH2CH2；R3 is (CH2) nCHOH, and n is one kind in 1-10 positive integer.
After the modifying agent is added in calcium carbonate powder, it is capable of dispersiveness of the improvement calcium carbonate of high degree in matrix material, makes
It is good with the compatibility of matrix material, improve the mechanical property of product so that impact strength significantly structural reform.
The calcium carbonate modifier, material composition is preferably in parts by weight 0.5 part of compound, 0.003 part of odium stearate, phosphorus
Sour 0.04 part of urea.Under the proportion relation so that after directly being mixed with calcium carbonate powder, be added into matrix material, prepare system
Product so that the mechanical property of product significantly improves.
It is preferred that described urea phosphate is after phosphoric acid is mixed with urea, to add water so that it is completely dissolved, and is placed in temperature
To act at 130-160 DEG C so that it forms (H2PO4)-(H2NCONH3)+Ion, and promote two particle effect 20-
30min, you can.So that dihydrogen phosphate ions and (H2NCONH3)+Ionic interaction, and mixed with compound, odium stearate
Afterwards, realize improves to the activity on calcium carbonate powder surface, reduces reunion rate, improves dispersiveness, improves and matrix material
Compatibility, improve the quality of product.
It is preferred that calcium carbonate modifier preparation method, comprises the following steps：
(1) urea phosphate is melted at 90-120 DEG C, and adds odium stearate, stirred, obtain just expecting；
(2) it is to be stirred under 100-300r/min by compound and just material low whipping speed, is placed in grinder, grinds
Mills, 600-800 mesh sieves are crossed, obtain modifier powder, you can.By melt process, odium stearate is added, and stir with compound
Mixing, grinding sieving are mixed, high degree causes the enhancing of modifier modification function so that after modified calcium carbonate powder, adds
Enter in matrix material, be prepared into product, larger amplitude occurs for its notch impact strength, tensile strength and tension failure strain etc.
The change of degree, it is capable of performance of the improvement calcium carbonate of high degree as filler.
In addition, this researcher also provides a kind of calcium carbonate modified method, comprises the following steps：
(1) by calcium carbonate grind into powder, water is added to be modulated into slurries, adjustment pH value is 11.0, is preheating to 40-50 DEG C；
(2) by above-mentioned calcium carbonate modifier, it is added to according to calcium carbonate powder quality 2-13% is accounted in slurries, at ultrasonic wave
10-20min is managed, spray drying, 300-600 mesh sieves is crossed, produces.
Described adjustment pH value is adjusted using aqua calcis.
Calcium carbonate after modification, it is added in resin material, is prepared into resin, it resists to product
There occurs high degree improvement for stretching, notch impact strength and tension failure strain etc. so that the mechanical property of product and comprehensive
Close performance and obtain improvement by a relatively large margin.
Specifically in order to verify that the modifying agent of the invention can be to calcium carbonate modified, as filler so that product properties
Change result, and this researcher has carried out following experiment：
Control 1：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 1
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 2：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 2
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 3：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 3
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 4：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 4
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 5：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 5
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 6：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 6
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 7：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 7
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 8：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 8
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 9：Paris white is accounted for according to calcium carbonate modifier using the calcium carbonate modifier and calcium carbonate powder of embodiment 9
Last quality 3% directly mixes, and after stirring, makees the filler of PVC product.
Control 10：It is modified to calcium carbonate powder according to the calcium carbonate modified method of embodiment 10, made PVC product
Filler.
Control 11：It is modified to calcium carbonate powder according to the calcium carbonate modified method of embodiment 11, made PVC product
Filler.
Control 12：It is modified to calcium carbonate powder according to the calcium carbonate modified method of embodiment 12, made PVC product
Filler.
Control 13：It is modified to calcium carbonate powder according to the calcium carbonate modified method of embodiment 13, made PVC product
Filler.
And the sample stretching of preparation and notched impact properties are tested, as a result as shown in table 1：
Table 1
| Notch impact strength (KJ/ ㎡) | Tensile strength (MPa) | Tension failure strains (%) | |
| Control 1 | 92.15 | 39.46 | 236.1 |
| Control 2 | 93.54 | 38.97 | 246.5 |
| Control 3 | 93.27 | 39.35 | 243.7 |
| Control 4 | 99.87 | 40.82 | 245.1 |
| Control 5 | 94.16 | 41.08 | 241.5 |
| Control 6 | 95.71 | 40.91 | 239.8 |
| Control 7 | 93.46 | 40.52 | 237.4 |
| Control 8 | 94.17 | 39.78 | 240.6 |
| Control 9 | 94.08 | 39.61 | 238.7 |
| Control 10 | 97.18 | 41.51 | 239.6 |
| Control 11 | 98.62 | 40.97 | 237.4 |
| Control 12 | 99.47 | 41.06 | 241.5 |
| Control 13 | 96.84 | 41.33 | 240.9 |
Above notch impact strength testing standard is GB/T1040-92；Above tensile strength and tension failure strain testing
Standard is GB/T1843-2008/ISO180：2000.
From upper table data, it can be seen that the calcium carbonate modifier of the invention is capable of the improvement carbonic acid of high degree
Calcium adds the mechanical property in PVC product as filler.
Embodiment
Limited with reference to specific embodiment technical scheme is further, but claimed
Scope is not only limited to made description.
Embodiment 1
A kind of calcium carbonate modifier, material composition is by weight compound 0.1kg, odium stearate 0.001kg, urea phosphate
0.01kg；Wherein molecular structure of compounds is：
Wherein, R1 is phenyl；R2 is methylene；R3 is (CH2) nCHOH, n 1.
Embodiment 2
A kind of calcium carbonate modifier, material composition is by weight compound 0.6kg, odium stearate 0.007kg, urea phosphate
0.06kg；Wherein molecular structure of compounds is：
Wherein, R1 is ether base；R2 is ethylidene；R3 is (CH2) nCHOH, n 10.
Embodiment 3
A kind of calcium carbonate modifier, material composition is by weight compound 0.5kg, odium stearate 0.002kg, urea phosphate
0.05kg；Wherein molecular structure of compounds is：
Wherein, R1 is vinyl；R2 is CH2CH2CH2OCH2CH2CH2；R3 is (CH2)
NCHOH, n 8.
Embodiment 4
A kind of calcium carbonate modifier, material composition is by weight compound 0.5kg, odium stearate 0.003kg, urea phosphate
0.04kg；Wherein molecular structure of compounds is：
Wherein, R1 is cycloalkyl；R2 is CH2CH2CH2OCH2CH2CH2；R3 is (CH2)
NCHOH, n 5.
Embodiment 5
On the basis of embodiment 1, urea phosphate is after phosphoric acid is mixed with urea, to add water so that it is completely dissolved, juxtaposition
It is to be acted at 130 DEG C in temperature so that it forms (H2PO4)-(H2NCONH3)+Ion, and promote two ionizations
20min, you can.
Embodiment 6
On the basis of embodiment 2, urea phosphate is after phosphoric acid is mixed with urea, to add water so that it is completely dissolved, juxtaposition
It is to be acted at 160 DEG C in temperature so that it forms (H2PO4)-(H2NCONH3)+Ion, and promote two ionizations
30min, you can.
Embodiment 7
On the basis of embodiment 1, calcium carbonate modifier preparation method, comprise the following steps：
(1) urea phosphate is melted at 90 DEG C, and adds odium stearate, stirred, obtain just expecting；
(2) it is to be stirred under 100r/min by compound and just material low whipping speed, is placed in grinder, grinds,
600 mesh sieves are crossed, obtain modifier powder, you can.
Embodiment 8
On the basis of embodiment 6, calcium carbonate modifier preparation method, comprise the following steps：
(1) urea phosphate is melted at 120 DEG C, and adds odium stearate, stirred, obtain just expecting；
(2) it is to be stirred under 300r/min by compound and just material low whipping speed, is placed in grinder, grinds,
800 mesh sieves are crossed, obtain modifier powder, you can.
Embodiment 9
On the basis of embodiment 5, calcium carbonate modifier preparation method, comprise the following steps：
(1) urea phosphate is melted at 100 DEG C, and adds odium stearate, stirred, obtain just expecting；
(2) it is to be stirred under 200r/min by compound and just material low whipping speed, is placed in grinder, grinds,
700 mesh sieves are crossed, obtain modifier powder, you can.
Embodiment 10
Calcium carbonate modified method, comprises the following steps：
(1) by calcium carbonate grind into powder, water is added to be modulated into slurries, sodium hydroxide adjustment pH value is 11.0, is preheating to 40
℃；
(2) by the calcium carbonate modifier of embodiment 1, it is added to according to calcium carbonate powder quality 2% is accounted in slurries, ultrasonic wave
10min is handled, spray drying, 300 mesh sieves is crossed, produces.
Embodiment 11
Calcium carbonate modified method, comprises the following steps：
(1) by calcium carbonate grind into powder, water is added to be modulated into slurries, calcium hydroxide adjustment pH value is 11.0, is preheating to 50
℃；
(2) by the calcium carbonate modifier of embodiment 2, it is added to according to calcium carbonate powder quality 13% is accounted in slurries, ultrasound
Ripple handles 20min, spray drying, crosses 600 mesh sieves, produces.
Embodiment 12
Calcium carbonate modified method, comprises the following steps：
(1) by calcium carbonate grind into powder, water is added to be modulated into slurries, potassium hydroxide adjustment pH value is 11.0, is preheating to 45
℃；
(2) by the calcium carbonate modifier of embodiment 6, it is added to according to calcium carbonate powder quality 8% is accounted in slurries, ultrasonic wave
15min is handled, spray drying, 400 mesh sieves is crossed, produces.
Embodiment 13
Calcium carbonate modified method, comprises the following steps：
(1) by calcium carbonate grind into powder, water is added to be modulated into slurries, aqua calcis adjustment pH value is 11.0, preheating
To 40 DEG C；
(2) by the calcium carbonate modifier of embodiment 9, it is added to according to calcium carbonate powder quality 13% is accounted in slurries, ultrasound
Ripple handles 10min, spray drying, crosses 600 mesh sieves, produces.
Claims (6)
1. a kind of calcium carbonate modifier, it is characterised in that material composition is in parts by weight compound 0.1-0.6 parts, stearic acid
Sodium 0.001-0.007 parts, urea phosphate 0.01-0.06 parts；Wherein molecular structure of compounds is：
Wherein, R1 is one kind in phenyl, ether base, vinyl, cycloalkyl；R2 is methylene, Asia
One kind in ethyl, CH2CH2CH2OCH2CH2CH2；R3 is (CH2) nCHOH, and n is one kind in 1-10 positive integer.
2. calcium carbonate modifier as claimed in claim 1, it is characterised in that described material composition is chemical combination in parts by weight
0.5 part of thing, 0.003 part of odium stearate, 0.04 part of urea phosphate.
3. calcium carbonate modifier as claimed in claim 1 or 2, it is characterised in that described urea phosphate is by phosphoric acid and urea
After mixing, add water so that it is completely dissolved, and it is to be acted at 130-160 DEG C to be placed in temperature so that it forms (H2PO4)-With
(H2NCONH3)+Ion, and promote two particle effect 20-30min, you can.
4. the calcium carbonate modifier preparation method as described in claim any one of 1-3, it is characterised in that comprise the following steps：
(1) urea phosphate is melted at 90-120 DEG C, and adds odium stearate, stirred, obtain just expecting；
(2) it is to be stirred under 100-300r/min by compound and just material low whipping speed, is placed in grinder, grinds,
600-800 mesh sieves are crossed, obtain modifier powder, you can.
A kind of 5. calcium carbonate modified method, it is characterised in that comprise the following steps：
(1) by calcium carbonate grind into powder, water is added to be modulated into slurries, adjustment pH value is 11.0, is preheating to 40-50 DEG C；
(2) modification for preparing any one of claim 1-3 calcium carbonate modifier or claim 4 preparation method, according to
Account for calcium carbonate powder quality 2-13% to be added in slurries, ultrasonication 10-20min, be spray-dried, cross 300-600 mesh sieves,
Produce.
6. calcium carbonate modified method as claimed in claim 5, it is characterised in that described adjustment pH value is to use calcium hydroxide
Solution adjusts.
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| CN108676409A (en) * | 2018-05-03 | 2018-10-19 | 安徽雪雨洁具有限公司 | A kind of heat-insulating, fire-preventing suitable for house ornamentation plank paints |
| CN109943195A (en) * | 2019-03-26 | 2019-06-28 | 马鞍山采石矶涂料有限公司 | A kind of preparation method of steel anticorrosive paint |
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Application publication date: 20180209 |