CN107915933A - A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic - Google Patents
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic Download PDFInfo
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- CN107915933A CN107915933A CN201711377693.6A CN201711377693A CN107915933A CN 107915933 A CN107915933 A CN 107915933A CN 201711377693 A CN201711377693 A CN 201711377693A CN 107915933 A CN107915933 A CN 107915933A
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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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- 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
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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
- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, and lime is mixed with tap water and carries out digestion reaction, and refined lime milk solution is obtained by screening out miscellaneous, standing；By lime milk solution than recanalization to 1.050 1.070, cooling, is delivered to the carbonization kettle with stirring, and is passed through purified kiln gas and carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, obtains nano-calcium carbonate slurries；Slurries are heated to, and are added fatty acid sodium salt and are carried out surface activation process, press filtration obtains filter cake；Filtration cakes torrefaction, crushes, and nano-calcium carbonate semi-finished product are made；Continuing modifier is finally delivered to, acrylamide styrol copolymer is added and haloflex carries out surface modification, you can obtain the toughened nano calcium carbonate product of the present invention.Nano-calcium carbonate prepared by the present invention has good processability and dispersiveness, can significantly improve the intensity and impact resistance of PVC plastic.
Description
Technical field
The present invention relates to nano-material modified technical field, is specifically a kind of special toughened nano calcium carbonate of PVC plastic
Preparation method.
Background technology
Polyvinyl chloride (PVC) has nonflammable, corrosion-resistant, insulation, wear-resistant, cheap, raw material sources are extensive etc.
Excellent comprehensive performance, is widely used in tubing, bar, film, insulating materials, anti-corrosion material, construction material etc., is
A kind of important thermoplastic, its yield are only second to polyethylene (PE) and occupy world's resin yield second.But make in PVC
During, the shortcomings of brittleness is big, heat endurance is poor, processing performance is bad is also exposed, performance is remained to be further improved and carried
It is high.
The activeness and quietness that nano-calcium carbonate is widely used in PVC plastic is modified, its nano particle is scattered in matrix continuous phase,
Macroscopical homogeneous, " island " linkage structure of Microphase Separation is formed, matrix can be induced and produce substantial amounts of shear band and crazing, so as to change
The impact resistance of kind PVC matrix.But found in practical application in industry, adding proportion one of the nano-calcium carbonate in PVC plastic
As no more than 15%, otherwise nano-calcium carbonate particles will be caused to reunite, obvious stress concentration is formed in matrix, caused multiple
The mechanical property of condensation material deteriorates.In addition, nano-calcium carbonate generally use aliphatic acid or soap progress table that industry is common
Face is modified, and not good enough with PVC matrix compatibility, the boundary layer between particle and matrix is weaker, and the modified effect of activeness and quietness extremely has
Limit.
Chinese invention patent CN 103468027A disclose a kind of modification side of the nano-calcium carbonate of hard PVC
Method, this method comprise the following steps：(1) nano-calcium carbonate is scattered in deionized water；(2) tristerin is added, after
It is continuous scattered；(3) filter and dry.The invention wraps the nano-calcium carbonate being scattered in liquid phase using tristerin
Cover, strengthen the lipophile of nano-calcium carbonate, although improving dispersiveness of the nano-calcium carbonate in polyvinyl chloride resin to a certain extent
With mobility, but the boundary strength between inorganic particulate and organic matrix is weaker, can not be effectively improved the mechanical property of PVC.
Chinese invention patent CN 105504881A disclose a kind of Nano calcium carbonate dedicated surface of PVC injection molding materials and are modified
Method, by specific surface area 20-32m2The calcium carbonate suspension slurry of/g, persistently stirs and is warming up to 70-90 DEG C, then add compound
Surface conditioning agent is coated, and stirring 60-90min completes surface treatment, cools down, filtering, be dry, pulverize to obtain surface and is modified and receives
Rice calcium carbonate product；The compound base amount method agent is alkylnaphthalene sulfonate and the blend of soap；Using this method
Though the nano-calcium carbonate calcium product of preparation can improve the appearance property of PVC rigid plastics, it can not realize the improvement of performance and carry
It is high.
The disclosure of background above technology contents is only used for inventive concept and the technical solution that auxiliary understands the present invention, it is not
The prior art of present patent application is necessarily belonged to, shows the applying date of the above in present patent application in no tangible proof
In the case of disclosed, above-mentioned background technology should not be taken to the novelty and creativeness of evaluation the application.
The content of the invention
The present invention for existing PVC plastic nano-calcium carbonate there are the problem of, there is provided a kind of PVC plastic is received with toughening type
When the preparation method of rice calcium carbonate, the nano-calcium carbonate being prepared of this method are used for PVC plastic and are modified, have it is good plus
Work and dispersiveness, can significantly improve the intensity and impact resistance of product.
In order to realize the above object the technical solution adopted by the present invention is as follows：
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, includes the following steps：
S1：Lime and tap water are pressed 1:The mass ratio of 4-6 carries out digestion reaction, after screening out miscellaneous, standing 24-48h
Obtain refined lime milk solution；
S2：By lime milk solution than recanalization to 1.050-1.070,18-22 DEG C is cooled to, is delivered to the carbonization with stirring
Kettle, and be passed through purified kiln gas and carry out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained
BET specific surface area is 18-30m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 60-95 DEG C, add fatty acid sodium salt, stir 20-
30min carries out surface activation process, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；
S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add calcium carbonate butt quality 0.1-0.5%'s
The haloflex of acrylamide-styrene copolymer and calcium carbonate butt quality 1.0-2.0%, modification temperature 120-140
DEG C, stir evenly, you can obtain the toughened nano calcium carbonate product of the present invention.
Further, the lime is the lime of activity degree >=380ml.
Further, the CO2 volumetric concentrations of the kiln gas are 25-35%.
Further, the soap is one kind in sodium laurate, Sodium myristate, sodium palmitate, odium stearate
Or the multiple combinations arbitrarily matched.
Further, the molecular weight of the acrylamide-styrene copolymer is 10000-50000.
Further, chlorinity is 35-40% in the haloflex.
Further, stirring described in step S3 and step S5 is stirred in the case where rotating speed is 100-300r/min.
Compared with prior art, advantages of the present invention and have the beneficial effect that：
1st, nano-calcium carbonate prepared by the present invention has good processability and dispersiveness, can significantly improve PVC plastic
Intensity and impact resistance.
2nd, the method for the present invention carries out nano-calcium carbonate using acrylamide-styrene copolymer and haloflex secondary
Dry method modification, after nano grain surface formation low pole caoutchouc elasticity clad, filled PVC plastics, these low poles cladding
Layer will form certain thickness boundary layer between the polar molecule of PVC, when being subject to external impacts, which plays buffering
Effect, effectively realizes toughening modifying function while intensity is not lost.
3rd, the method for the present invention technique simple possible, production cost is low, and energy consumption is low, and there is preferable economic benefit and society to imitate
Benefit.
Embodiment
The present invention is described in further detail with reference to embodiment.It is emphasized that the description below is only
Only it is exemplary, the scope being not intended to be limiting of the invention and its application.
Embodiment 1
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, includes the following steps：
S1：The lime of activity degree >=380ml and tap water are pressed 1:4 mass ratio carries out digestion reaction, through screening out it is miscellaneous,
Refined lime milk solution is obtained after standing 24h；
S2：By lime milk solution than recanalization to 1.050,19 DEG C are cooled to, is delivered to the carbonization kettle with stirring, and be passed through
Purified kiln gas carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained BET and compared surface
Product is 29.3m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 85 DEG C, adds and is for calcium carbonate butt quality
2.0% odium stearate, 30min progress surface activation process is stirred in the case where rotating speed is 150r/min, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；
S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add the propylene of calcium carbonate butt quality 0.5%
(chlorinity is for acid amides-styrol copolymer (molecular weight 20000) and the haloflex of calcium carbonate butt quality 2.0%
37%), modification temperature is 130 DEG C, is stirred evenly in the case where rotating speed is 150r/min, you can obtain the toughened nano carbon of the present invention
Sour calcium.
Embodiment 2
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, includes the following steps：
S1：The lime of activity degree >=380ml and tap water are pressed 1:5 mass ratio carries out digestion reaction, through screening out it is miscellaneous,
Refined lime milk solution is obtained after standing 36h；
S2：By lime milk solution than recanalization to 1.055,18 DEG C are cooled to, is delivered to the carbonization kettle with stirring, and be passed through
Purified kiln gas carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained BET and compared surface
Product is 24.7m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 90 DEG C, adds and is for calcium carbonate butt quality
1.7% sodium laurate, 20min progress surface activation process is stirred in the case where rotating speed is 300r/min, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；
S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add the propylene of calcium carbonate butt quality 0.3%
(chlorinity is for acid amides-styrol copolymer (molecular weight 50000) and the haloflex of calcium carbonate butt quality 1.5%
35%), modification temperature is 120 DEG C, is stirred evenly in the case where rotating speed is 300r/min, you can obtain the toughened nano carbon of the present invention
Sour calcium.
Embodiment 3
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, includes the following steps：
S1：The lime of activity degree >=380ml and tap water are pressed 1:5 mass ratio carries out digestion reaction, through screening out it is miscellaneous,
Refined lime milk solution is obtained after standing 48h；
S2：By lime milk solution than recanalization to 1.065,22 DEG C are cooled to, is delivered to the carbonization kettle with stirring, and be passed through
Purified kiln gas carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained BET and compared surface
Product is 18.6m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 90 DEG C, adds and is for calcium carbonate butt quality
1.0% sodium laurate, 25min progress surface activation process is stirred in the case where rotating speed is 300r/min, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；
S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add the propylene of calcium carbonate butt quality 0.5%
(chlorinity is for acid amides-styrol copolymer (molecular weight 10000) and the haloflex of calcium carbonate butt quality 1.8%
40%), modification temperature is 130 DEG C, is stirred evenly in the case where rotating speed is 300r/min, you can obtain the toughened nano carbon of the present invention
Sour calcium.
Embodiment 4
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, includes the following steps：
S1：The lime of activity degree >=380ml and tap water are pressed 1:6 mass ratio carries out digestion reaction, through screening out it is miscellaneous,
Refined lime milk solution is obtained after standing 30h；
S2：By lime milk solution than recanalization to 1.070,18 DEG C are cooled to, is delivered to the carbonization kettle with stirring, and be passed through
Purified kiln gas carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained BET and compared surface
Product is 22.6m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 70 DEG C, adds and is for calcium carbonate butt quality
1.8% sodium laurate, 30min progress surface activation process is stirred in the case where rotating speed is 150r/min, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；
S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add the propylene of calcium carbonate butt quality 0.4%
(chlorinity is for acid amides-styrol copolymer (molecular weight 30000) and the haloflex of calcium carbonate butt quality 1.0%
35%), modification temperature is 120 DEG C, is stirred evenly in the case where rotating speed is 150r/min, you can obtain the toughened nano carbon of the present invention
Sour calcium.
Embodiment 5
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, includes the following steps：
S1：The lime of activity degree >=380ml and tap water are pressed 1:6 mass ratio carries out digestion reaction, through screening out it is miscellaneous,
Refined lime milk solution is obtained after standing 36h；
S2：By lime milk solution than recanalization to 1.060,20 DEG C are cooled to, is delivered to the carbonization kettle with stirring, and be passed through
Purified kiln gas carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained BET and compared surface
Product is 26.1m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 90 DEG C, adds and is for calcium carbonate butt quality
2.0% odium stearate, 20min progress surface activation process is stirred in the case where rotating speed is 300r/min, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；
S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add the propylene of calcium carbonate butt quality 0.3%
(chlorinity is for acid amides-styrol copolymer (molecular weight 20000) and the haloflex of calcium carbonate butt quality 1.5%
35%), modification temperature is 130 DEG C, is stirred evenly in the case where rotating speed is 300r/min, you can obtain the toughened nano carbon of the present invention
Sour calcium.
Embodiment 6
A kind of preparation method of the special toughened nano calcium carbonate of PVC plastic, includes the following steps：
S1：The lime of activity degree >=380ml and tap water are pressed 1:5 mass ratio carries out digestion reaction, through screening out it is miscellaneous,
Refined lime milk solution is obtained after standing 36h；
S2：By lime milk solution than recanalization to 1.065,22 DEG C are cooled to, is delivered to the carbonization kettle with stirring, and be passed through
Purified kiln gas carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained BET and compared surface
Product is 28.9m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 90 DEG C, adds and is for calcium carbonate butt quality
1.5% Sodium myristate, 30min progress surface activation process is stirred in the case where rotating speed is 150r/min, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；
S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add the propylene of calcium carbonate butt quality 0.3%
(chlorinity is for acid amides-styrol copolymer (molecular weight 40000) and the haloflex of calcium carbonate butt quality 1.0%
40%), modification temperature is 130 DEG C, is stirred evenly in the case where rotating speed is 150r/min, you can obtain the toughened nano carbon of the present invention
Sour calcium.
Comparative example
This comparative example difference from Example 1 is that the preparation method of comparative example nano-calcium carbonate comprises the following steps：
S1：The lime of activity degree >=380ml and tap water are pressed 1:4 mass ratio carries out digestion reaction, through screening out it is miscellaneous,
Refined lime milk solution is obtained after standing 24h；
S2：By lime milk solution than recanalization to 1.050,19 DEG C are cooled to, is delivered to the carbonization kettle with stirring, and be passed through
Purified kiln gas carries out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, is obtained BET and compared surface
Product is 29.3m2The nano-calcium carbonate slurries of/g；
S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 85 DEG C, adds and is for calcium carbonate butt quality
4.5% odium stearate, 30min progress surface activation process is stirred in the case where rotating speed is 150r/min, and press filtration obtains filter cake；
S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate is made.
Nano-calcium carbonate prepared by above example 1-6 of the present invention and comparative example prepares PVC plastic by formula as below respectively.
Each raw material is weighed according to following ratio of weight and number：SG-5100 parts of PVC, 5.0 parts of calcium zinc stabilizer, 0.5 part of stearic acid, polyethylene
4.0 parts of 0.5 part of wax, 35 parts of nano-calcium carbonate, 2.0 parts of ACR and titanium dioxide.It is kneaded in advance in high-speed mixer by formula
20min, is granulated and is molded through double screw extruder and injection molding machine respectively, obtains PVC plastic test sample.
Properties of product test is carried out to above-mentioned PVC plastic test sample, GB/T1040.2- is pressed in wherein tensile strength test
Method as defined in 2006 carries out；Impact strength method as defined in GB/T 1043.1-2006 carries out, the test result such as institute of table 1
Show：
Table 1：Nano-calcium carbonate prepared by the present invention is applied to the properties of product for preparing PVC plastic
The nano-calcium carbonate of the present invention is can be seen that from above-mentioned experiment, compared to the nano-sized carbon of normal fat hydrochlorate processing
Sour calcium, has more preferable mechanical property, especially impact resistance in PVC plastic.
Above content is to combine specific/preferred embodiment further description made for the present invention, it is impossible to
Assert that the specific implementation of the present invention is confined to these explanations.Come for general technical staff of the technical field of the invention
Say, without departing from the inventive concept of the premise, it can also make some replacements or modification to the embodiment that these have been described,
And these are substituted or variant is regarded as belonging to protection scope of the present invention.
Claims (7)
- A kind of 1. preparation method of the special toughened nano calcium carbonate of PVC plastic, it is characterised in that：Include the following steps：S1：Lime and tap water are pressed 1:The mass ratio of 4-6 carries out digestion reaction, is obtained after screening out miscellaneous, standing 24-48h Refined lime milk solution；S2：By lime milk solution than recanalization to 1.050-1.070,18-22 DEG C is cooled to, is delivered to the carbonization kettle with stirring, And be passed through purified kiln gas and carry out carbonation reaction, until reaction system pH ＜ 7.3, carbonation reaction is completed, that is, obtains BET Specific surface area is 18-30m2The nano-calcium carbonate slurries of/g；S3：The nano-calcium carbonate slurries that step S2 is obtained are heated to 60-95 DEG C, add fatty acid sodium salt, stir 20- 30min carries out surface activation process, and press filtration obtains filter cake；S4：By above-mentioned filtration cakes torrefaction, crush, nano-calcium carbonate semi-finished product are made；S5：Nano-calcium carbonate semi-finished product are delivered to continuing modifier, add the propylene of calcium carbonate butt quality 0.1-0.5% The haloflex of acid amides-styrol copolymer and calcium carbonate butt quality 1.0-2.0%, modification temperature are 120-140 DEG C, are stirred Mix uniformly, you can obtain the toughened nano calcium carbonate product of the present invention.
- 2. the preparation method of the special toughened nano calcium carbonate of PVC plastic according to claim 1, it is characterised in that：It is described Lime is the lime of activity degree >=380ml.
- 3. the preparation method of the special toughened nano calcium carbonate of PVC plastic according to claim 1, it is characterised in that：It is described The CO2 volumetric concentrations of kiln gas are 25-35%.
- 4. the preparation method of the special toughened nano calcium carbonate of PVC plastic according to claim 1, it is characterised in that：It is described Soap is sodium laurate, Sodium myristate, sodium palmitate, one kind in odium stearate or the multiple combinations arbitrarily matched.
- 5. the preparation method of the special toughened nano calcium carbonate of PVC plastic according to claim 1, it is characterised in that：It is described The molecular weight of acrylamide-styrene copolymer is 10000-50000.
- 6. the preparation method of the special toughened nano calcium carbonate of PVC plastic according to claim 1, it is characterised in that：It is described Chlorinity is 35-40% in haloflex.
- 7. the preparation method of the special toughened nano calcium carbonate of PVC plastic according to claim 1, it is characterised in that：Step Stirring described in S3 and step S5 is stirred in the case where rotating speed is 100-300r/min.
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Cited By (4)
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| CN110791040A (en) * | 2019-11-01 | 2020-02-14 | 连州市凯恩斯纳米材料有限公司 | Nano calcium carbonate for toughening PVC (polyvinyl chloride) and preparation method thereof |
| CN110878164A (en) * | 2019-06-14 | 2020-03-13 | 安徽鑫豪爵新材料科技有限公司 | PVC floor film with scratch self-repairing function and production process thereof |
| CN110982301A (en) * | 2019-11-01 | 2020-04-10 | 连州市凯恩斯纳米材料有限公司 | Nano calcium carbonate with plasticizing function and preparation method thereof |
| CN114316631A (en) * | 2021-12-28 | 2022-04-12 | 广西华纳新材料科技有限公司 | Functionalized nano calcium carbonate for hard PVC |
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